THEREOF

CROSS-REFERENCE

[001] This application claims the benefit of U.S. Provisional Application No. 61/514,149, filed August 2, 2011, which application is incorporated herein by reference.

FIELD OF THE INVENTION

[002] Described herein are beryllium oxide compounds and films, substantially pure beryllium compounds and methods for preparing the same, and sublimation devices.

BACKGROUND OF THE INVENTION

[003] Disubstituted beryllium compounds are used in a variety of applications, including the preparation of beryllium oxide films.

SUMMARY OF THE INVENTION

[004] Disclosed herein is beryllium oxide prepared from a substantially pure disubstituted beryllium product. In some embodiments, the substantially pure disubstituted beryllium product is produced by any of the methods described herein. In some embodiments, the beryllium oxide is in the form of a beryllium oxide film.

[005] In some embodiments, beryllium oxide is prepared from a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct. In some embodiments, the beryllium oxide is in the form of a film. In some embodiments, a beryllium oxide film is prepared from a disubstituted beryllium product, wherein the disubstituted beryllium product is a sublimed or otherwise purified disubstituted beryllium product. In some embodiments, a beryllium oxide film is prepared via a vapor deposition process from a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct.

[006] In some embodiments, a beryllium oxide film is prepared from dialkyl beryllium, diaryl beryllium, alkylaryl beryllium, dihalogen beryllium, arylhalogen beryllium, or alkylhalogen beryllium. In some embodiments, a beryllium oxide film is prepared from dimethyl beryllium. In some embodiments, a beryllium oxide film is prepared from a disubstituted beryllium product comprising hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups. In some embodiments, a beryllium oxide film is prepared from a disubstituted beryllium product that is differentially substituted with groups selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, and halogen groups.

[007] In some embodiments, a beryllium oxide film is produced that contains bulk properties of high thermal conductivity and high thermal stability. [008] In another aspect, a beryllium oxide film is produced by oxidizing the disubstituted beryllium product prepared by any of the methods described herein. In another aspect, a beryllium oxide film is produced by hydrolyzing the disubstituted beryllium product prepared by any of the methods described herein.

[009] In another aspect, a beryllium oxide film is produced via a vapor deposition process from the disubstituted beryllium product prepared by the methods described herein.

[010] In some embodiments of the beryllium oxide film, the beryllium oxide film is prepared from a disubstituted beryllium compound that contains 5% or less of impure disubstituted beryllium.

[011] In some embodiments of the beryllium oxide film, the film contains bulk properties of high thermal conductivity and high thermal stability.

[012] In some embodiments of the beryllium oxide film, the film is prepared from a disubstituted beryllium compound that contains 5% or less of disubstituted beryllium diethyl etherate. In some embodiments of the beryllium oxide film, the film is prepared from a dialkyl beryllium compound that contains 5% or less of impure dialkyl beryllium. In some embodiments of the beryllium oxide film, the film is prepared from dimethyl beryllium that contains 5% or less of impure dimethyl beryllium. In some embodiments of the beryllium oxide film, the film is prepared from dimethyl beryllium that contains 5% or less of dimethyl beryllium diethyl etherate. In some embodiments of the beryllium oxide film, the film is prepared from diethyl beryllium that contains 5% or less of impure diethyl beryllium. In some embodiments of the beryllium oxide film, the film is prepared from diethyl beryllium that contains 5% or less of diethyl beryllium diethyl etherate.

[013] In some embodiments of the beryllium oxide film, the thermal conductivity is 300W/mk. In some embodiments of the beryllium oxide film, the dielectric constant is 6.8. In some embodiments of the beryllium oxide film, the binding energy is in the range of 1113 to 1115 eV.

[014] Further described herein is a sublimed disubstituted beryllium product that is at least 95% free of a beryllium-Lewis base adduct.

[015] Further described herein is a sublimed dimethyl beryllium product that is at least 95% free of a beryllium-Lewis base adduct.

[016] Also described herein are substantially pure disubstituted beryllium compounds that contain 5% or less of a beryllium-Lewis base adduct and methods for preparing the same. In some embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium comprises hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups. In some embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium is differentially substituted with groups selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups. In some

embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium is dialkyl beryllium, diaryl beryllium, alkylaryl beryllium, dihalogen beryllium, arylhalogen beryllium, or alkylhalogen beryllium. In one embodiment, dimethyl beryllium is produced that contains 5% or less of a beryllium-Lewis base adduct.

[017] In some embodiments, the beryllium-Lewis base adduct is a beryllium etherate. In some embodiments, the beryllium etherate is selected from the group consisting of disubstituted beryllium etherate, disubstituted beryllium dialkyl etherate, disubstituted beryllium diethyl etherate, disubstituted beryllium dibutyl etherate, dialkyl beryllium dialkyl etherate, dialkyl beryllium diethyl etherate, dialkyl beryllium dibutyl etherate, dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dimethyl beryllium dibutyl etherate, and diethyl beryllium dibutyl etherate, or a combination thereof.

[018] Also described herein is a method of providing substantially pure disubstituted beryllium, comprising: purifying an impure disubstituted beryllium product with the aid of a sublimation vessel or via distillation or via other methods of purification to provide a disubstituted beryllium product that is substantially free of impure disubstituted beryllium.

[019] Also described herein is a method of providing a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct, comprising purifying an impure disubstituted beryllium product with the aid of a sublimation vessel or via distillation, or other methods of purification.

[020] In some embodiments of the methods described herein, the impure disubstituted beryllium product is a disubstituted beryllium compound that contains greater than 5% of a beryllium-Lewis base adduct.

[021] In some embodiments of the methods described herein, the beryllium-Lewis base adduct is a beryllium etherate. In some embodiments of the methods described herein, the impure disubstituted beryllium product is dimethyl beryllium containing greater than 5% of dimethyl beryllium diethyl etherate.

[022] Also disclosed herein is a method for purifying the impure disubstituted beryllium product by sublimation with the aid of a sublimation vessel. In some embodiments of the methods described herein, the sublimation vessel heats the impure disubstituted beryllium product in a uniform manner.

[023] In some embodiments of the methods described herein, the sublimation vessel comprises: a bottom surface and a surrounding wall extending upward from the bottom surface to form a main chamber with one opening; wherein the main chamber houses a heating chamber comprising at least one compartment enclosed by a surrounding wall; wherein the heating chamber is not in communication with the main chamber and has at least one opening for the introduction of heating fluid for heating the main chamber.

[024] In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 0°C to about 300°C. In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a pressure ranging from less than 1 millitorr to about 760 millitorr. In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 0°C to about 300°C under reduced pressure. In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 0°C to about 300°C under high dynamic vacuum.

[025] In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 0°C to about 300°C at a pressure between about 5 to about 10 millitorr.

[026] In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 75°C to about 160°C. In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 75°C to about 160°C under reduced pressure. In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 75°C to about 160°C under high dynamic vacuum In some embodiments of the methods described herein, sublimation of the disubstituted beryllium occurs at a temperature ranging from about 75 °C to about 160°C at a pressure between about 5 to about 10 millitorr.

[027] In some embodiments of the methods described herein, sublimation of dimethyl beryllium occurs at a temperature ranging from about 75°C to about 160°C. In some embodiments of the methods described herein, sublimation of dimethyl beryllium occurs at a temperature ranging from about 75 °C to about 160°C under reduced pressure. In some embodiments of the methods described herein, sublimation of dimethyl beryllium occurs at a temperature ranging from about 75°C to about 160°C under high dynamic vacuum. In some embodiments of the methods described herein, sublimation of dimethyl beryllium occurs at a temperature ranging from about 75°C to about 160°C at a pressure between about 5 to about 10 millitorr.

[028] In some embodiments of the methods described herein, the sublimation is repeated multiple times.

[029] In some embodiments, a purified disubstituted beryllium is produced that contains 5% or less of impure disubstituted beryllium. In some embodiments, the purified disubstituted beryllium product contains 5% or less of disubstituted beryllium diethyl etherate. In some embodiments, the purified disubstituted beryllium product contains 5% or less of disubstituted beryllium dibutyl etherate.

[030] In some embodiments, a purified disubstituted beryllium is produced that contains 5% or less of a dialkyl beryllium diethyl etherate. In some embodiments, the purified disubstituted beryllium product contains 5% or less of a dialkyl beryllium dibutyl etherate.

[031] In some embodiments, the purified disubstituted beryllium product contains 5% or less of dimethyl beryllium diethyl etherate. In some embodiments, the purified disubstituted beryllium product contains 5% or less of diethyl beryllium diethyl etherate. In some embodiments, the purified disubstituted beryllium product contains 5% or less of dimethyl beryllium dibutyl etherate. In some embodiments, the purified disubstituted beryllium product contains 5% or less of diethyl beryllium dibutyl etherate. [032] In some embodiments, the purified dialkyl beryllium product contains 5% or less of dialkyl beryllium diethyl etherate. In some embodiments, purified dimethyl beryllium is produced that contains 5% or less of dimethyl beryllium diethyl etherate. In some embodiments, purified diethyl beryllium is produced that contains 5% or less of diethyl beryllium diethyl etherate.

[033] In some embodiments, a disubstituted beryllium is produced that contains 5% or less of a beryllium-Lewis base adduct. In some embodiments, the beryllium-Lewis base adduct is a beryllium etherate. In some embodiments, the beryllium etherate is selected from the group consisting of disubstituted beryllium etherate, disubstituted beryllium dialkyl etherate, disubstituted beryllium diethyl etherate, disubstituted beryllium dibutyl etherate, dialkyl beryllium dialkyl etherate, dialkyl beryllium diethyl etherate, dialkyl beryllium dibutyl etherate, dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dimethyl beryllium dibutyl etherate, and diethyl beryllium dibutyl etherate, or a combination thereof.

[034] In some embodiments, a disubstituted beryllium that contains 5% or less of a beryllium-Lewis base adduct is produced that comprises hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups.

[035] In some embodiments, a disubstituted beryllium that contains 5% or less of a beryllium-Lewis base adduct is produced wherein the disubstituted beryllium is differentially substituted with groups selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl,

heterocycloalkyl, or halogen groups.

[036] In some embodiments, a disubstituted beryllium that contains 5% or less of a beryllium-Lewis base adduct is produced wherein the disubstituted beryllium is dialkyl beryllium, diaryl beryllium, alkylaryl beryllium, dihalogen beryllium, arylhalogen beryllium, or alkylhalogen beryllium.

In some embodiments, a disubstituted beryllium that contains 5% or less of a beryllium-Lewis base adduct is produced wherein the disubstituted beryllium is dimethyl beryllium.

[037] Also disclosed herein is a method for preparing the impure disubstituted beryllium product, comprising reacting a beryllium substrate and an organometallic reagent in solvent.

[038] In some embodiments of the methods described herein, the beryllium substrate is a beryllium dihalide. In some embodiments, the beryllium substrate is beryllium dichloride.

[039] In some embodiments of the methods described herein, the organometallic reagent is an organomagnesium or organolithium reagent. In some embodiments of the methods described herein, the organometallic reagent is an organomagnesium reagent comprising aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups. In some embodiments of the methods described herein, the organometallic reagent is an organomagnesium halide. In some embodiments, the organometallic reagent is an organomagnesium bromide or an organomagnesium chloride. In some embodiments, the organometallic reagent is an organomagnesium bromide. In some embodiments, the organometallic reagent is an organomagnesium chloride. In some embodiments, the organometallic reagent is an organomagnesium iodide. [040] In some embodiments of the methods described herein, the organometallic reagent is a methylmagnesium halide. In some embodiments, the organometallic reagent is methylmagnesium bromide. In some embodiments, the organometallic reagent is methylmagnesium chloride. In some embodiments, the organometallic reagent is methylmagnesium iodide. In some embodiments of the methods described herein, the organometallic reagent is an ethylmagnesium halide. In some

embodiments, the organometallic reagent is ethylmagnesium bromide. In some embodiments, the organometallic reagent is ethylmagnesium chloride. In some embodiments, the organometallic reagent is ethylmagnesium iodide. In some embodiments of the methods described herein, the organometallic reagent is propylmagnesium bromide. In some embodiments, the organometallic reagent is

propylmagnesium chloride. In some embodiments, the organometallic reagent is propylmagnesium iodide. In some embodiments of the methods described herein, the organometallic reagent is phenylmagnesium bromide. In some embodiments, the organometallic reagent is phenylmagnesium chloride. In some embodiments, the organometallic reagent is phenylmagnesium iodide.

[041] In some embodiments of the methods described herein, the organometallic reagent is an organo lithium reagent comprising aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups. In some embodiments of the methods described herein, the organometallic reagent is methyllithium. In some embodiments of the methods described herein, the organometallic reagent is ethyllithium. In some embodiments of the methods described herein, the organometallic reagent is propyllithium. In some embodiments of the methods described herein, the organometallic reagent is phenyllithium.

[042] In some embodiments of the methods described herein, the solvent is an aprotic and nonaqueous solvent. In some embodiments of the methods described herein, the solvent is optionally selected from tetrahydrofuran, alkyl-substituted tetrahydrofuran, dioxane, toluene, pentane, hexanes, dialkyl ether, cycloalkanes, diethoxymethane, or butyl diglyme.

[043] In some embodiments of the methods described herein, the solvent is a mixture of two or more aprotic, nonaqueous solvents. In some embodiments of the methods described herein, the solvent is a mixture of two or more solvents optionally selected from tetrahydrofuran, alkyl-substituted

tetrahydrofuran, dioxane, toluene, pentane, hexanes, dialkyl ether, cycloalkanes, diethoxymethane, or butyl diglyme. In some embodiments of the methods described herein, the solvent is diethyl ether. In some embodiments of the methods described herein, the solvent is dibutyl ether. In some embodiments of the methods described herein, the solvent is tetrahydrofuran. In some embodiments of the methods described herein, the solvent is 2-methyltetrahydrofuran. In some embodiments of the methods described herein, the solvent is a mixture of tetrahydrofuran and toluene. In some embodiments of the methods described herein, the solvent is substantially free from oxygen.

[044] In some embodiments of the methods described herein, a solution of the impure disubstituted beryllium product is filtered to remove inorganic salts. In some embodiments of the methods described herein, a solution of the impure disubstituted beryllium product is filtered over dry Celite to remove inorganic salts. In some embodiments of the methods described herein, a solution of the impure disubstituted beryllium product is filtered over dry Celite to remove magnesium salts. In some embodiments of the methods described herein, a solution of the impure disubstituted beryllium product is filtered over dry Celite to remove lithium salts.

[045] In some embodiments of the methods described herein, the bulk solvent is removed from the impure disubstituted beryllium product. In some embodiments of the methods described herein, the impure disubstituted beryllium product is concentrated to dryness. In some embodiments of the methods described herein, the bulk solvent is removed from the impure disubstituted product under high performance vacuum. In some embodiments, the impure disubstituted beryllium product is concentrated to dryness under high performance vacuum. In some embodiments of the methods described herein, the bulk solvent is removed from the impure disubstituted beryllium product at a pressure between about 5 to about 10 millitorr.

[046] In some embodiments of the methods described herein, the disubstituted beryllium comprises groups optionally selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups.

[047] In some embodiments of the methods described herein, the disubstituted beryllium is differentially substituted with groups optionally selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups.

[048] In some embodiments of the methods described herein, the disubstituted beryllium comprises two aryl groups. In some embodiments of the methods described herein, the disubstituted beryllium comprises two alkyl groups. In some embodiments of the methods described herein, the disubstituted beryllium is dimethyl beryllium. In some embodiments of the methods described herein, the disubstituted beryllium is diethyl beryllium. In some embodiments of the methods described herein, the disubstituted beryllium is dipropyl beryllium. In some embodiments of the methods described herein, the disubstituted beryllium is diphenyl beryllium.

[049] In another aspect, a sublimation vessel is described herein, comprising: a bottom surface and a surrounding wall extending upward from the bottom surface to form a main chamber with one opening; wherein the main chamber houses a heating chamber comprising at least one compartment enclosed by a surrounding wall; wherein the heating chamber is not in communication with the main chamber and has at least one opening for the introduction of heating fluid for heating the main chamber.

[050] In another aspect, a heating chamber for use in sublimation is described herein comprising a chimney sealed to a turbo tube to form a chamber with at least two compartments, wherein the chimney comprises a glass tube flattened on one end with an opening in its base for the introduction of heating fluid, and the turbo tube comprises any suitable glass tube with an opening for the introduction or exit of heating fluid.

[051] In some embodiments of the sublimation vessel, the heating chamber of the sublimation vessel has more than one opening for the introduction or exit of heating fluid. In some embodiments of the sublimation vessel, the heating chamber has one opening in the bottom surface of the vessel. In some embodiments of the sublimation vessel, a compartment of the heating chamber traverses the main chamber, such that there is an interspace between the bottom surface of the vessel and the compartment.

[052] In some embodiments of the sublimation vessel, the surrounding wall of the heating chamber is nonporous.

[053] In some embodiments of the sublimation vessel, the surrounding wall of the heating chamber is nonporous such that no gas exchange is possible between the heating chamber and the main chamber. In some embodiments of the sublimation vessel, the surrounding wall of the heating chamber is nonporous such that no fluid exchange is possible between the heating chamber and the main chamber. In some embodiments of the sublimation vessel, the heating chamber comprises multiple compartments. In some embodiments of the sublimation vessel, the heating chamber comprises an array of interconnected compartments. In some embodiments of the sublimation vessel, the heating chamber comprises an array of vertical and horizontal compartments.

[054] In some embodiments of the sublimation vessel, the sublimation vessel further comprises a collection plate. In some embodiments, the collection plate is removable. In some embodiments, the collection plate can be removed via a handle attached to the plate without inversion of the vessel. In some embodiments, the collection plate sits upon the heating chamber. In some embodiments, the collection plate is porous. In some embodiments, the porosity of the collection plate is such that a gas can pass through it. In some embodiments, the collection plate is nonporous. In some embodiments, gas can pass around the collection plate.

[055] In some embodiments of the sublimation vessel, the vessel is made of any type of glass suitable for heating and cooling. In some embodiments of the sublimation vessel, the vessel is made of any type of glass suitable for heating and cooling under reduced pressure. In some embodiments of the sublimation vessel, the vessel is made of any type of glass suitable for heating and cooling under vacuum.

[056] In some embodiments of the sublimation vessel, the vessel is made of borosilicate glass.

[057] In some embodiments of the sublimation vessel, the top of the vessel further comprises a flange.

[058] In some embodiments of the sublimation vessel, the vessel further comprises a condenser, wherein the vessel is connected to the condenser. In some embodiments of the sublimation vessel, the condenser and vessel have mating flanges. In some embodiments of the sublimation vessel, the condenser and vessel are connected via an O-ring joint. In some embodiments of the sublimation vessel, the O-ring joint consists of a top flange that is ground flat and a bottom mating flange that has a groove for an O-ring. In some embodiments of the sublimation vessel, the condenser and vessel are connected with the aid of a clamp. In some embodiments of the sublimation vessel, the condenser further comprises a port for connecting the condenser to a mechanical pump, vacuum pump, manifold or Schlenk line.

[059] In some embodiments of the sublimation vessel, a port is attached to the wall surrounding the main chamber for connecting the vessel to a mechanical pump, vacuum pump, or Schlenk line. [060] In some embodiments of the sublimation vessel, the capacity of the main chamber is anywhere between less than 1 milliliter to multiple liters.

[061] In some embodiments of the methods described herein, the sublimation vessel described herein is used for the purification of disubstituted beryllium.

[062] In another embodiment, the sublimation vessel described herein is used to provide disubstituted beryllium that is substantially free of impure disubstituted beryllium. In another embodiment, the sublimation vessel described herein is used to provide disubstituted beryllium that contains 5% or less of a beryllium-Lewis base adduct.

[063] In some embodiments of the heating chamber assembly, the chimney comprises an outer diameter between about 1 mm and about 420 mm. In some embodiments of the heating chamber assembly, the chimney comprises an outer diameter between about 1 mm and about 75 mm. In some embodiments of the heating chamber assembly, the chimney comprises an outer diameter of about 25 mm.

[064] In some embodiments of the heating chamber assembly, the turbo tube comprises an outer diameter between about 1 mm to about 420 mm. In some embodiments of the heating chamber assembly, the turbo tube comprises an outer diameter of about 12 mm to about 15 mm. In some embodiments of the heating chamber assembly, the turbo tube is sealed to the chimney at about a 90 degree angle. In some embodiments of the heating chamber assembly, multiple turbo tubes are sealed to the chimney. In some embodiments of the heating chamber assembly, three turbo tubes are sealed to the chimney. In some embodiments of the heating chamber assembly, the turbo tubes are separated from one another by about 120 degrees. In some embodiments of the heating chamber assembly, four turbo tubes are sealed to the chimney. In some embodiments of the heating chamber assembly, the turbo tubes are separated from one another by about 90 degrees.

[065] In some embodiments of the heating chamber assembly, the chimney comprises glass optionally selected from borosilicate glass; ambered glass; or quartz. In one embodiment, the chimney comprises borosilicate glass. In one embodiment, the chimney comprises Type I, class A, borosilicate glass.

[066] In some embodiments of the heating chamber assembly, the turbo tube comprises glass optionally selected from borosilicate glass; ambered glass; or quartz. In one embodiment of the heating chamber assembly, the turbo tube comprises borosilicate glass. In one embodiment, the turbo tube comprises Type I, class A, borosilicate glass.

[067] In some embodiments of the heating chamber assembly, the turbo tube is in communication with the chimney. In some embodiments of the heating chamber assembly, the turbo tube is connected to the chimney such that fluid exchange is possible between them. In some embodiments of the heating chamber assembly, the turbo tube is not in communication with the chimney. In some embodiments of the heating chamber assembly, fluid exchange between the chimney and the turbo tube is not possible via the juncture of the turbo tube and chimney. INCORPORATION BY REFERENCE

[068] All publications, patents, and patent applications mentioned in this specification are herein incorporated by reference to the same extent as if each individual publication, patent, or patent application was specifically and individually indicated to be incorporated by reference. BRIEF DESCRIPTION OF THE FIGURES

[069] The novel features of the invention are set forth with particularity in the appended claims. A better understanding of the features and advantages of the present invention will be obtained by reference to the following detailed description that sets forth illustrative embodiments, in which the principles of the invention are utilized, and the accompanying figures of which:

[070] FIGURE 1 shows an example of a sublimation vessel with a heating chamber according to an embodiment of the current disclosure.

[071] FIGURE 2 shows an example of the base of a sublimation vessel with a heating chamber according to an embodiment of the current disclosure.

[072] FIGURE 3 shows an example of a sublimation vessel, a collection plate, and a condenser according to an embodiment of the current disclosure.

[073] FIGURE 4 shows an example of a sublimation vessel, a collection plate, an O-ring, a clamp, and a condenser, according to an embodiment of the current disclosure.

[074] FIGURE 5 shows an example of a sublimation vessel connected to a condenser via an O-ring joint and a clamp, along with a collection plate sitting upon the heating chamber, according to an embodiment of the current disclosure.

[075] FIGURE 6 shows a magnified example of a sublimation vessel connected to a condenser with an O-ring joint and a clamp, along with a collection plate sitting upon the heating chamber, according to an embodiment of the current disclosure.

[076] FIGURE 7 shows an example of a normal sublimation vessel produced by Chemglass, catalog no. CG-3038.

[077] FIGURE 8 shows an example of a normal sublimation vessel produced by Aldrich, catalog no. Z129593.

DETAILED DESCRIPTION OF THE INVENTION

[078] Currently available methods of preparing disubstituted beryllium compounds result in disubstituted beryllium products that are contaminated with impurities, which cannot be substantially removed using current purification methods. Consequently, substantially pure disubstituted beryllium compounds cannot be made using current methods. This is important because many desirable products, including beryllium oxide, are prepared from disubstituted beryllium and the purity of the disubstituted beryllium significantly impacts the quality of the beryllium oxide, i.e., a less pure disubstituted beryllium yields a beryllium oxide product of inferior quality. [079] Researchers in the field have assumed that producing disubstituted beryllium compounds of very high purity is not achievable. The Applicants recognized that the present invention could produce disubstituted beryllium compounds of very high purity, which in turn would lead to beryllium oxide compounds of superior quality that are not obtainable using current methods. One solution identified by the Applicants is the use of uniform heating of the purification apparatus.

[080] Sublimation is a common method of purifying chemical compounds. However, the use of sublimation vessels known in the prior art yields sublimed products that are contaminated with impurities. This is particularly problematic when the compound that needs to be purified contains impurities that have sublimation temperatures that are close to the sublimation temperature of the desired compound. This problem is illustrated in example 2 herein, wherein dimethyl beryllium is sublimed using a normal sublimation vessel, and the resultant sublimed dimethyl beryllium is contaminated with dimethyl beryllium diethyl etherate. ^l H NMR analysis of several different batches of sublimed product shows that about 2.0 to about 0.5 molecules of diethyl ether are coordinated to every molecule of dimethyl beryllium. In example 2 described herein, the dimethyl beryllium is prepared as follows: In a nitrogen filled glovebox, a 500 mL Schlenk flask is charged with BeC . (15 g, 188 mmol). The BeCLJs dissolved in cold (-30 °C) and dry diethyl ether (125 mL), which results in the formation of a turbid solution. To this solution, 128.25 mL of MeMgBr (3 M in diethyl ether, 386 mmol) is added in a dropwise manner. The resulting cloudy suspension is stirred in the glovebox for 16 hours and then is filtered over dry Celite to remove precipitated magnesium salts. The ethereal solution is concentrated to dryness on a high performance vacuum line. The obtained solid residue is transferred into a normal sublimation vessel, with an attached condenser, wherein the dimethyl beryllium is sublimed multiple times. This procedure is repeated multiple times and dimethyl beryllium that is contaminated with dimethyl beryllium diethyl etherate is consistently obtained. ^l H NMR analysis of several different batches of sublimed product shows that about 2.0 to about 0.5 molecules of diethyl ether are coordinated to every molecule of dimethyl beryllium.

[081] The present invention overcomes the problem illustrated by example 2 by using the custom sublimation vessel described herein. Example 1 illustrates one embodiment of the presently disclosed solution for producing a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct. In the example 1 described herein, substantially pure dimethyl beryllium is prepared as follows: In a nitrogen filled glovebox, a 500 mL Schlenk flask is charged with BeC . (15 g, 188 mmol). The BeCi ₂ is dissolved in cold (-30 °C) and dry diethyl ether (125 mL), which results in the formation of a turbid solution. To this solution, 128.25 mL of MeMgBr (3 M in diethyl ether, 386 mmol) is added in a dropwise manner. The resulting cloudy suspension is stirred in the glovebox for 16 hours and then is filtered over dry Celite to remove precipitated magnesium salts. The ethereal solution is concentrated to dryness on a high performance vacuum line. The obtained solid residue is transferred into the custom sublimation vessel, with an attached condenser, wherein it is heated slowly from ambient temperature to 150 °C under high dynamic vacuum When the oil bath temperature reaches about 85 °C, the product begins to sublime. The sublimation is repeated multiple times to afford pure BeMe ₂ . ^ι ΐΙ NMR analysis indicates that the BeMe ₂ is greater than or equal to 95% pure.

Definitions

[082] "Alkenyl" refers to a group that begins with the atoms -C(R)=C(R)-R, wherein R refers to the remaining portions of the alkenyl group, which are optionally the same or different. The alkenyl moiety may be acyclic or cyclic. Alkenyl groups are optionally substituted. Non-limiting examples of an alkenyl group include -C(CH ₃ )=CH ₂ , -CH=CHCH ₃ ,and the like.

[083] "Alkynyl" refers to a group that begins with the atoms -C≡C(R), wherein R refers to the remaining portions of the alkynyl group. Alkynyl groups are optionally substituted. Non-limiting examples of an alkenyl group include -C≡CH, -C≡CCH ₃ , -C≡CCH ₂ CH ₃ , -C≡CCH ₂ CH ₂ CH ₃ , and the like.

[084] "Allyl" means a radical. The alkenyl and allylic carbons of the allyl groups are optionally substituted. Non-limiting examples of an allyl group include -C(H)=C(H)-CH ₂ -,

-C(CH ₃ )=C(H)-CH ₂ - -C(CH ₃ )=C(CH ₃ )-CH ₂ - -C(CH ₃ )=C(H)-C(CH ₃ )H- and the like.

[085] "Alkyl" refers to a saturated, aliphatic hydrocarbon. The alkyl moiety is optionally branched or straight chain. Alkyl groups are optionally substituted with non-alkyl groups, such as aryl, alkenyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups. Non-limiting examples of an alkyl include methyl, ethyl, propyl, and the like.

[086] "Aryl" means a monovalent monocyclic or bicyclic aromatic hydrocarbon radical of 6 to 10 ring atoms e.g., napthyl or phenyl.

[087] "Cycloalkyl" means a cyclic saturated monovalent hydrocarbon radical of 3 to 10 carbon atoms, e.g., cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, and the like. Cycloalkyl groups are optionally substituted.

[088] "Dialkyl beryllium dibutyl etherate" means a compound of the type BeR ₂ »(OBu ₂ ) _x , wherein "x" refers to the number of ether molecules complexed or coordinated to the beryllium, R is an alkyl group, and the two R groups are optionally the same or different, "x" does not have to be an integer. Non- limiting examples include dimethyl beryllium dibutyl etherate, diethyl beryllium dibutyl etherate, dipropyl beryllium dibutyl etherate, methylethyl beryllium dibutyl etherate and the like.

[089] "Dialkyl beryllium diethyl etherate" means a compound of the type BeR ₂ »(OEt ₂ ) _x , wherein "x" refers to the number of ether molecules complexed or coordinated to the beryllium, R is an alkyl group, and the two R groups are optionally the same or different, "x" does not have to be an integer. Non- limiting examples include dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dipropyl beryllium diethyl etherate, and the like.

[090] "Disubstituted beryllium" means a compound of the type BeR ₂ , wherein the two R groups are optionally the same or different and comprise hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups. Non-limiting examples include dimethyl beryllium, diethyl beryllium, dipropyl beryllium, diphenyl beryllium, methylethyl beryllium and the like.

[091] "Disubstituted beryllium dibutyl etherate" means a compound of the type BeR ₂ »(OBu ₂ ) _x , wherein "x" refers to the number of ether molecules complexed or coordinated to the beryllium, and R is optionally the same or different. R is optionally selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups, "x" does not have to be an integer. Non-limiting examples include dimethyl beryllium dibutyl etherate, diethyl beryllium dibutyl etherate, dipropyl beryllium dibutyl etherate, diphenyl beryllium dibutyl etherate, and the like.

[092] "Disubstituted beryllium diethyl etherate" means a compound of the type BeR ₂ »(OEt ₂ ) _x , wherein "x" refers to the number of ether molecules complexed or coordinated to the beryllium, and R is optionally the same or different. R is optionally selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups, "x" does not have to be an integer. Non- limiting examples include dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dipropyl beryllium diethyl etherate, diphenyl beryllium diethyl etherate, and the like.

[093] "Ethyl" group means a -CH ₂ CH ₃ radical.

[094] "Heteroaryl" means a monovalent monocyclic or bicyclic aromatic radical of 5 to 10 ring atoms where one or more ring atoms are a heteroatom selected from N, O, or S, the remaining ring atoms being carbon. Representative examples include, but are not limited to, pyrrolyl, thienyl, thiazolyl, imidazolyl, furanyl, indolyl, isoindolyl, oxazolyl, isoxazolyl, benzothiazolyl, benzoxazolyl, quinolinyl, isoquinolinyl, pyridinyl, pyrimidinyl, pyrazinyl, pyridazinyl, triazolyl, tetrazolyl, and the like.

[095] "Heterocycloalkyl" means a saturated or unsaturated monovalent monocyclic group of 4 to 8 ring atoms in which one or more ring atoms are a heteroatom selected from N, O, or S, the remaining ring atoms being C.

[096] "High dynamic vacuum" means any pressure less than about 0.01 mm Hg (torr).

[097] "Lewis base" refers to a chemical species capable of providing a pair of electrons and thus capable of forming an adduct with a Lewis acid.

[098] "Methyl" group means a -CH ₃ radical.

[099] "Normal sublimation vessel" means a sublimation vessel that is commonly used by one skilled in the art for sublimation. Non-limiting examples of normal sublimation vessels include sublimation vessels that are commercially available, e.g., sublimation apparatus, catalog number CG-3038, sold by Chemglass (shown in Fig. 7) and sublimation apparatus, catalog number Z129593, sold by Aldrich (shown in Fig. 8) .

[0101] "Propyl" group mean a -CH ₂ CH ₂ CH ₃ radical.

[0102] "Reduced pressure" means any pressure less than about 760 mmHg (torr). [0103] "Sublimate" means a purified product obtained by subliming a less pure product. "Sublimate" is used interchangeably with "sublimed product."

[0104] "Substantially pure" means containing minimal amounts of an impurity.

[0105] "Vessel" means a container, e.g., flask, beaker.

[0106] "Vinyl" means a -CH=CH ₂ radical.

[0107] In some embodiments, deuterated analogs of the disubstituted beryllium compounds are optionally prepared. In some embodiments, deuterated analogs of the organometallic reagents are optionally used. In some embodiments, a deuterated solvent is optionally used. Semiconductive materials and films prepared from pure disubstituted beryllium compounds

[0108] In one aspect of this invention, the disubstituted beryllium product prepared by any of the methods described herein is suitable for the production of desirable materials or compounds. In some embodiments, the disubstituted beryllium product prepared by any of the methods described herein is suitable for use in the production of semiconductor materials, compounds, or films.

[0109] In another aspect of this invention, a beryllium oxide film is produced. In some embodiments, a beryllium oxide film is produced by oxidizing or hydrolyzing the disubstituted beryllium product prepared by any of the methods described herein.

[0110] In another aspect of this invention, a beryllium oxide film is deposited in layers onto a metal device. In some embodiments, a beryllium oxide film produced from the disubstituted beryllium product prepared by any of the methods described herein is deposited in layers onto a metal device. In some embodiments, a beryllium oxide film produced by oxidizing or hydrolyzing the disubstituted beryllium product prepared by any of the methods described herein is deposited in layers onto a metal device.

[0111] In another aspect of this invention, beryllium oxide produced from the disubstituted beryllium product prepared by any of the methods described herein is optionally used in a variety of applications including, but not limited to, molecular electronics; conductive polymers; gate dielectrics; insulators; light- emitting diodes; interfacial passivation layer applications; field-effect transistors; solar cells; chips; photovoltaic cells; gas diffusion applications; or anti-corrosion barrier applications.

[0112] In another aspect, beryllium oxide produced from the disubstituted beryllium product prepared by any of the methods described herein is optionally mixed with a second conductive or semiconductive material for use in a variety of applications including, but not limited to, molecular electronics;

conductive polymers; gate dielectrics; insulators; light- emitting diodes; interfacial passivation layer applications; field-effect transistors; solar cells; chips; photovoltaic cells; gas diffusion applications; or anti-corrosion barrier applications.

[0113] In another aspect, a beryllium oxide film is produced via a vapor deposition process from the disubstituted beryllium product prepared by the methods described herein. [0114] In some embodiments of the beryllium oxide film, the film contains a bulk property of high thermal conductivity. In some embodiments of the beryllium oxide film, the film contains a bulk property of high thermal stability.

[0115] In some embodiments of the beryllium oxide film, the beryllium oxide film is prepared from a disubstituted beryllium compound that contains 5% or less of impure disubstituted beryllium. In some embodiments of the beryllium oxide film, the film is prepared from a disubstituted beryllium compound that contains 5% or less of a beryllium-Lewis base adduct. In some embodiments of the beryllium oxide film, the film is prepared from a disubstituted beryllium compound that contains 5% or less of disubstituted beryllium diethyl etherate. In some embodiments of the beryllium oxide film, the film is prepared from a dialkyl beryllium compound that contains 5% or less of impure dialkyl beryllium.

[0116] In some embodiments of the beryllium oxide film, the film is prepared from dimethyl beryllium that contains 5% or less of impure dimethyl beryllium.

[0117] In some embodiments of the beryllium oxide film, the film is prepared from dimethyl beryllium that contains 5% or less of dimethyl beryllium diethyl etherate. In some embodiments of the beryllium oxide film, the film is prepared from diethyl beryllium that contains 5% or less of impure diethyl beryllium. In some embodiments of the beryllium oxide film, the film is prepared from diethyl beryllium that contains 5% or less of diethyl beryllium diethyl etherate.

[0118] In some embodiments of the beryllium oxide film, the thermal conductivity is 300W/mk. In some embodiments of the beryllium oxide film, the dielectric constant is 6.8. In some embodiments of the beryllium oxide film, the binding energy is in the range of 1113 to 1115 eV.

Substantially pure disubstituted beryllium compounds

[0119] Also described herein are substantially pure disubstituted beryllium compounds that contain 5% or less of a beryllium-Lewis base adduct. In some embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium comprises hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups. In some embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium is differentially substituted with groups selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl, heterocycloalkyl, or halogen groups. In some embodiments, a disubstituted beryllium product that contains 5% or less of a beryllium-Lewis base adduct is produced, wherein the disubstituted beryllium is dialkyl beryllium, diaryl beryllium, alkylaryl beryllium, dihalogen beryllium, arylhalogen beryllium, or alkylhalogen beryllium. In one embodiment, dimethyl beryllium is produced that contains 5% or less of a beryllium-Lewis base adduct.

[0120] Further described herein is a sublimed disubstituted beryllium product that is at least 95% free of a beryllium-Lewis base adduct. Further described herein is a sublimed dimethyl beryllium product that is at least 95% free of a beryllium-Lewis base adduct. [0121] In some embodiments, the beryllium-Lewis base adduct is a beryllium etherate. In some embodiments, the beryllium etherate is selected from the group consisting of disubstituted beryllium etherate, disubstituted beryllium dialkyl etherate, disubstituted beryllium diethyl etherate, disubstituted beryllium dibutyl etherate, dialkyl beryllium dialkyl etherate, dialkyl beryllium diethyl etherate, dialkyl beryllium dibutyl etherate, dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dimethyl beryllium dibutyl etherate, and diethyl beryllium dibutyl etherate, or a combination thereof.

[0122] In an aspect of this invention, disubstituted beryllium is provided that contains a minimal amount of an impurity. In some embodiments of this invention, disubstituted beryllium is provided that contains a minimal amount of a beryllium impurity. In some embodiments of this invention, disubstituted beryllium is provided that contains a minimal amount of impure disubstituted beryllium. In some embodiments, disubstituted beryllium is provided that is about 95% pure. In some embodiments, disubstituted beryllium is provided that is greater than 95% pure. In some embodiments, disubstituted beryllium is provided that is greater than 96%, 97%, 98%, or 99% pure.

[0123] In some embodiments, disubstituted beryllium is provided that contains about 5% or less of an impurity. In some embodiments, the purified disubstituted beryllium product contains about 5% or less of an impure disubstituted beryllium. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of an impurity. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of an impure disubstituted beryllium. In some

embodiments, the sublimed disubstituted beryllium product contains about 5% or less of a beryllium impurity.

[0124] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of a beryllium-Lewis base adduct. In some embodiments, the Lewis base in the beryllium-Lewis base adduct is a solvent that contains a Lewis basic site. In some embodiments, the Lewis base in the beryllium- Lewis base adduct is an ethereal solvent. In some embodiments, the Lewis base in the beryllium-Lewis base adduct is diethyl ether, dibutyl ether, tetrahydrofuran, tert-butyl methyl ether, 2- methyltetrahydrofuran, butyl diglyme, dioxane, anisole, cyclopentyl methyl ether, dioxolane, alkyl- substituted tetrahydrofuran, tetrahydropyran, dialkyl ether, diisopropyl ether, dimethoxyethane, diethoxymethane, or diglyme, or a combination thereof.

[0125] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of a disubstituted beryllium diethyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of a disubstituted beryllium diethyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of a disubstituted beryllium diethyl etherate.

[0126] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of a disubstituted beryllium dibutyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of a disubstituted beryllium dibutyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of a disubstituted beryllium dibutyl etherate.

[0127] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate.

[0128] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of a dialkyl beryllium dibutyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of a dialkyl beryllium dibutyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of a dialkyl beryllium dibutyl etherate.

[0129] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of dimethyl beryllium diethyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of dimethyl beryllium diethyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of dimethyl beryllium diethyl etherate.

[0130] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of diethyl beryllium diethyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of diethyl beryllium diethyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of diethyl beryllium diethyl etherate.

[0131] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of dimethyl beryllium dibutyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of dimethyl beryllium dibutyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of dimethyl beryllium dibutyl etherate.

[0132] In some embodiments, the purified disubstituted beryllium product contains about 5% or less of diethyl beryllium dibutyl etherate. In some embodiments, the sublimed disubstituted beryllium product contains about 5% or less of diethyl beryllium dibutyl etherate. In some embodiments, the distilled disubstituted beryllium product contains about 5% or less of diethyl beryllium dibutyl etherate.

[0133] In some embodiments, the purified dialkyl beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate. In some embodiments, the sublimed dialkyl beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate. In some embodiments, the distilled dialkyl beryllium product contains about 5% or less of a dialkyl beryllium diethyl etherate.

[0134] In some embodiments, the purified dimethyl beryllium product contains about 5% or less of the dimethyl beryllium diethyl etherate. In some embodiments, the sublimed dimethyl beryllium product contains about 5% or less of a dimethyl beryllium diethyl etherate. In some embodiments, the distilled dimethyl beryllium product contains about 5% or less of a dimethyl beryllium diethyl etherate.

[0135] In some embodiments, the purified diethyl beryllium product contains about 5% or less of a diethyl beryllium diethyl etherate. In some embodiments, the sublimed diethyl beryllium product contains about 5% or less of a diethyl beryllium diethyl etherate. In some embodiments, the distilled diethyl beryllium product contains about 5% or less of a diethyl beryllium diethyl etherate.

[0136] In some embodiments, the ratio of the disubstituted beryllium to the disubstituted beryllium impurity is greater than or equal to about 95:5. In some embodiments, the ratio of the dialkyl beryllium to the dialkyl beryllium impurity is greater than or equal to about 95:5. In some embodiments, the ratio of dimethyl beryllium to the dimethyl beryllium impurity is greater than or equal to about 95:5. In some embodiments, the ratio of the diethyl beryllium to the diethyl beryllium impurity is greater than or equal to about 95:5.

[0137] In one embodiment, the ratio of dimethyl beryllium to dimethyl beryllium diethyl etherate is greater than or equal to about 95:5. In one embodiment, the ratio of diethyl beryllium to diethyl beryllium diethyl etherate is greater than or equal to about 95:5.

[0138] In some embodiments, the disubstituted beryllium impurity is a beryllium-solvent complex, including, but not limited to, dimethyl beryllium diethyl etherate, diethyl beryllium diethyl etherate, dimethyl beryllium dibutyl etherate, diethyl beryllium dibutyl etherate, diphenyl beryllium diethyl etherate, diphenyl beryllium dibutyl etherate, dipropyl beryllium diethyl etherate, or dipropyl beryllium dibutyl etherate, or a combination thereof.

[0139] In some embodiments, the beryllium impurity is a beryllium oligomer.

[0140] In some embodiments, the purity of the disubstituted beryllium product is determined by ^l H

NMR analysis.

Methods of Purification

[0141] In an aspect of this invention, substantially pure disubstituted beryllium compounds are obtained via purification of an impure disubstituted beryllium compound. In some embodiments, the impure disubstituted beryllium compound is prepared by any of the methods disclosed herein. In some embodiments, the impure disubstituted beryllium product is purified via sublimation or distillation or another method of purification.

[0142] In some embodiments, the impure disubstituted beryllium product is purified via sublimation with the aid of a sublimation vessel. In some embodiments, the impure disubstituted beryllium product is purified via sublimation with the aid of a sublimation vessel that heats the impure disubstituted beryllium product uniformly. In one embodiment, the impure disubstituted beryllium product is purified via sublimation with the aid of a sublimation vessel described in Figures 1 through 6.

[0143] In some embodiments, the sublimation of the disubstituted beryllium product is achieved at a pressure ranging from about less than one millitorr to about 760 millitorr. In some embodiments, the sublimation of the disubstituted beryllium product is achieved under reduced pressure.

[0144] In some embodiments, the sublimation of the disubstituted beryllium product is achieved at a temperature ranging from about 0 °C to about 300 °C. In some embodiments, the sublimation of the disubstituted beryllium product is achieved at a temperature ranging from about 0 °C to about 300 °C. In some embodiments, the sublimation of the disubstituted beryllium product is achieved under reduced pressure at a temperature ranging from about 0 °C to about 300 °C.

[0145] In some embodiments, the sublimation of the disubstituted beryllium product is achieved under high dynamic vacuum. In some embodiments, the sublimation of the disubstituted beryllium product is achieved under high dynamic vacuum at a temperature ranging from about 0 °C to about 300 °C.

[0146] In some embodiments, the sublimation of the disubstituted beryllium product is achieved at atmospheric pressure. In some embodiments, the sublimation of the disubstituted beryllium product is achieved at atmospheric pressure at a temperature ranging from about 0 °C to about 300 °C.

[0147] In some embodiments, sublimation of the disubstituted beryllium product is achieved at a temperature ranging from about 75 °C to about 160 °C. In some embodiments, sublimation of the disubstituted beryllium product is achieved under reduced pressure at a temperature ranging from about 75 °C to about 160 °C.

[0148] In some embodiments, sublimation of the disubstituted beryllium product is achieved under high dynamic vacuum at a temperature ranging from about 75 °C to about 160 °C.

[0149] In some embodiments, sublimation of dimethyl beryllium is achieved under reduced pressure. In some embodiments, the sublimation of dimethyl beryllium is achieved under high dynamic vacuum. In one embodiment, sublimation of dimethyl beryllium is achieved under high dynamic vacuum at a temperature ranging from about 75 °C to about 160 °C.

[0150] In some embodiments, the sublimation is repeated. In some embodiments, the sublimation is repeated multiple times.

Preparation of impure disubstituted beryllium compounds

[0151] In an aspect of the invention, impure disubstituted beryllium compounds are prepared by reacting a beryllium substrate and an organometallic reagent in solvent.

Beryllium Substrate

[0152] In some embodiments, the beryllium substrate comprises a substituted beryllium compound. In some embodiments, the beryllium substrate is optionally selected from beryllium, beryllium chloride, beryllium bromide, beryllium iodide, or beryllium fluoride.

[0153] In some embodiments, the beryllium substrate is purchased from a commercial supplier. In some embodiments, the beryllium substrate is used as purchased from the commercial supplier. In some embodiments, the beryllium substrate is used as purchased without further purification.

[0154] In some embodiments the beryllium substrate is used as a solution. In some embodiments, the beryllium substrate is used as a solution in an aprotic solvent. In some embodiments, the beryllium substrate is used as a solution in a nonaqueous solvent. In some embodiments, the beryllium substrate is used as a solution in an aprotic and nonaqueous solvent.

[0155] In some embodiments, the aprotic and nonaqueous solvent is benzene, chlorobenzene, dichlorobenzene, trichlorobenzene, anisole, chlorobutane, trimethylpentane, methylbutane, diethyl ether, dibutyl ether, tertbutyl methyl ether, cyclopentyl methyl ether, dichloromethane, dioxane, dioxolane, tetrahydrofuran, 2-methyltetrahydrofuran, alkyl-substituted tetrahydrofuran, tetrahydropyran, toluene, hexanes, cyclohexane, methylcyclohexane, pentane, dialkyl ether, diisopropyl ether, cycloalkane, dimethoxyethane, diethoxymethane, diglyme, or butyl diglyme, or a combination thereof. In some embodiments, the beryllium substrate is used as a solution in diethyl ether. In some embodiments, the beryllium substrate is used as a solution in tetrahydrofuran. In some embodiments, the beryllium substrate is used as a solution in dioxane.

[0156] In some embodiments, the beryllium substrate is used as a solution at a temperature below about 23 °C. In some embodiments, the beryllium substrate is dissolved in an aprotic and nonaqueous solvent at a temperature below about 23 °C. In some embodiments, the solution of the beryllium substrate is prepared at a temperature below about 23 °C.

[0157] In some embodiments, the solution of the beryllium substrate is prepared at about -30 °C. In some embodiments, the beryllium substrate is dissolved in an aprotic and nonaqueous solvent at about - 30 °C. In some embodiments, the beryllium substrate is used as a solution in diethyl ether at about -30 °C.

OrganometalUc Reagent

[0158] In an aspect of this invention, an organometallic reagent is used. In some embodiments, the organometallic reagent comprises hydrogen, aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups. In some embodiments, the organometallic reagent is an organomagnesium or organolithium reagent comprising aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups.

[0159] In some embodiments of this invention, the organometallic reagent is an organomagnesium halide comprising aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups, e.g., methylmagnesium bromide, methylmagnesium iodide, methylmagnesium chloride, ethylmagnesium bromide, ethylmagnesium iodide, ethylmagnesium chloride, ethynylmagnesium bromide, ethynylmagnesium iodide, ethynylmagnesium chloride, vinylmagnesium bromide, vinylmagnesium iodide, vinylmagnesium chloride, 1 -propynylmagnesium bromide, 1- propynylmagnesium iodide, 1 -propynylmagnesium chloride, allylmagnesium bromide, allylmagnesium iodide, allylmagnesium chloride, cyclopropylmagnesium bromide, cyclopropylmagnesium iodide, cyclopropylmagnesium chloride, isoprenylmagnesium bromide, isoprenylmagnesium iodide, isoprenylmagnesium chloride, isopropylmagnesium bromide, isopropylmagnesium iodide,

isopropylmagnesium chloride, propylmagnesium bromide, propylmagnesium iodide, propylmagnesium chloride, 2-thienylmagnesium bromide, 2-thienylmagnesium iodide, 2-thienylmagnesium chloride, 3- thienylmagnesium bromide, 3-thienylmagnesium iodide, 3-thienylmagnesium chloride, (l,3-Dioxolan-2- ylmethyl)magnesium bromide, (l,3-Dioxolan-2-ylmethyl)magnesium iodide, (l,3-Dioxolan-2- ylmethyl)magnesium chloride, phenylmagnesium bromide, phenylmagnesium iodide, phenylmagnesium chloride, cyclohexylmagnesium bromide, cyclohexylmagnesium iodide, cyclohexylmagnesium chloride, butylmagnesium bromide, buylmagnesium iodide, butylmagnesium chloride, 3-butenylmagnesium bromide, 3-butenylmagnesium iodide, 3-butenylmagnesium chloride, 1 -methyl- 1 -propenylmagnesium bromide, 1 -methyl- 1 -propenylmagnesium iodide, or 1 -methyl- 1 -propenylmagnesium chloride.

[0160] In some embodiments, the organometallic reagent is used as a solution. In some embodiments, the organometallic reagent is used as a solution in an aprotic solvent, e.g., diethyl ether, dibutyl ether, tetrahydrofuran, tetrahydrofuran and toluene mixture, tert-butyl methyl ether, 2-methyltetrahydrofuran, butyl diglyme, dioxane, benzene, dichloromethane, or toluene. In some embodiments, the organometallic reagent is used as a solution in a nonaqueous solvent. In some embodiments, the organometallic reagent is used in a nonaqueous, aprotic solvent optionally selected from diethyl ether, dibutyl ether,

tetrahydrofuran, tetrahydrofuran and toluene mixture, tert-butyl methyl ether, 2-methyltetrahydrofuran, butyl diglyme, dioxane, benzene, dichloromethane, or toluene.

[0161] In some embodiments, the organomagnesium halide is used as a solution. In some embodiments, the organomagnesium halide is used as a solution in an aprotic solvent, e.g., diethyl ether, dibutyl ether, tetrahydrofuran, tetrahydrofuran and toluene mixture, tert-butyl methyl ether, 2-methyltetrahydrofuran, butyl diglyme, dioxane, benzene, dichloromethane, toluene, benzene, chlorobenzene, dichlorobenzene, trichlorobenzene, anisole, chlorobutane, trimethylpentane, methylbutane, cyclopentyl methyl ether, dichloromethane, dioxolane, alkyl-substituted tetrahydrofuran, tetrahydropyran, toluene, hexanes, cyclohexane, methylcyclohexane, pentane, heptane, dialkyl ether, diisopropyl ether, cycloalkane, dimethoxyethane, diethoxymethane, or diglyme, or a combination thereof. In some embodiments, the organomagnesium halide is used as a solution in a nonaqueous solvent. In some embodiments, the organomagnesium halide is used as a solution in an aprotic and nonaqueous solvent. In some embodiments, the organomagnesium halide is used in a solvent optionally selected from diethyl ether, dibutyl ether, tetrahydrofuran, tetrahydrofuran and toluene mixture, tert-butyl methyl ether, 2- methyltetrahydrofuran, butyl diglyme, dioxane, benzene, dichloromethane, or toluene.

[0162] In some embodiments, the organomagnesium halide is purchased from a commercial supplier. In some embodiments, the organomagnesium halide is used as purchased from the commercial supplier. In some embodiments, the organomagnesium halide is used as purchased without further purification.

[0163] In some embodiments, the organometallic reagent is synthesized. In some embodiments, the organomagnesium reagent is synthesized. In some embodiments, the organomagnesium halide is synthesized.

[0164] In some embodiments, the organometallic reagent is an organolithium. In some embodiments, the organometallic reagent is an organolithium comprising aryl, alkyl, alkenyl, vinyl, allyl, alkynyl, cycloalkyl, heteroaryl, or heterocycloalkyl groups, e.g., methyllithium, ethyllithium, propyllithium, isopropyllithium, vinyllithium, butyllithium, pentylhthium, phenyllithium, 2-furyllithium, 3-furyllithium, 2-thienyllithium, 3-thienyllithium, benzofuranyllithium, methyllithium lithium iodide complex, methyllithium lithium bromide, isobutyllithium, sec-butyllithium, tert-butyllithium, lithium

phenylacetylide, neopentyllithium, lithium(trimethylsilyl)acetylide, cyclopentadienyllithium, (trimethylsilyl)methyllithium, lithium acetylide ethylenediamine complex, 2-(ethylhexyl)lithium, lithium tetramethylcyclopentadienide, or lithium pentamethylcyclopentadienide.

[0165] In some embodiments, the organolithium is purchased from a commercial supplier. In some embodiments, the organolithium is used as purchased from the commercial supplier. In some embodiments, the organolithium is used as purchased without further purification.

[0166] In some embodiments the organolithium is synthesized.

Solvent

[0167] In some embodiments, disubstituted beryllium is prepared by reacting a beryllium substrate and an organometallic reagent in a suitable solvent.

[0168] In some embodiments, a suitable solvent is any solvent that does not react with the

organometallic reagent. In some embodiments, a suitable solvent is any solvent that does not react with the beryllium substrate. In some embodiments, a suitable solvent is an aprotic solvent. In some embodiments, a suitable solvent is an aprotic solvent. In some embodiments, a suitable solvent is a nonaqueous solvent. In some embodiments, a suitable solvent is a solvent that is substantially free from oxygen. In some embodiments, a suitable solvent is any solvent that is aprotic, nonaqueous, and substantially free from oxygen.

[0169] In one embodiment, a dialkyl ether solvent is used, e.g., diethyl ether, dibutyl ether, tert-butyl methyl ether and the like.

[0170] In some embodiments, the solvent is diethyl ether, dibutyl ether, tetrahydroiuran, tetrahydroiuran and toluene mixture, tert-butyl methyl ether, 2-methyltetrahydrofuran, butyl diglyme, dioxane, benzene, dichloromethane, toluene, benzene, chlorobenzene, dichlorobenzene, trichlorobenzene, anisole, chlorobutane, trimethylpentane, methylbutane, cyclopentyl methyl ether, dichloromethane, dioxolane, alkyl-substituted tetrahydroiuran, tetrahydropyran, toluene, hexanes, cyclohexane, methylcyclohexane, pentane, heptane, dialkyl ether, diisopropyl ether, cycloalkane, dimethoxyethane, diethoxymethane, or diglyme, or a combination thereof.

[0171] In some embodiments, a mixture of suitable solvents is used. In some embodiments, a mixture of aprotic, nonaqueous solvents is used, e.g., a 1 :1 mixture of toluene and tetrahydroiuran.

Stoichiometry and Concentration

[0172] In some embodiments, the beryllium substrate is used in excess of the organometallic reagent. In some embodiments, the organometallic reagent is used in excess of the beryllium substrate. In some embodiments, the beryllium substrate and organometallic reagent are used in a molar ratio of about 1 :1.

In one embodiment, the molar ratio of beryllium substrate to the organometallic reagent is about 1 :2.

[0173] In some embodiments, the concentration of the beryllium substrate in solvent is anywhere between about 0.1M to about 2M.

[0174] In one embodiment, the concentration of the beryllium substrate in solvent is about 1.5M.

[0175] In some embodiments, the concentration of the organometallic reagent in solvent is anywhere between about 0.1M and about 4M. [0176] In one embodiment, the concentration of the organometallic reagent in solvent is about 3M.

Reaction Temperature

[0177] In some embodiments, the reaction temperature is anywhere between about -78 °C to about 200 °C.

[0178] In some embodiments, the reaction temperature is maintained below about 23 °C. In some embodiments, the reaction temperature is maintained below about 23 °C during the addition of the organometallic reagent to the beryllium substrate.

[0179] In some embodiments, the reaction temperature is maintained at about -30 °C. In one embodiment, the reaction temperature is maintained at about -30 °C during the addition of the organometallic reagent to the beryllium substrate.

[0180] In some embodiments, the reaction temperature is raised over the course of the reaction. In some embodiments, the reaction temperature is slowly raised from about -78 °C to about 23 °C over the course of the reaction. In one embodiment, the reaction temperature is slowly raised from about -30 °C to about 23 °C over the course of the reaction.

Atmosphere

[0181] In some embodiments, the preparation of the impure disubstituted beryllium product is performed under an inert atmosphere. In some embodiments, the preparation of the impure disubstituted beryllium product is performed under an atmosphere that is substantially free from oxygen. In some embodiments, the preparation of the impure disubstituted beryllium product is performed under an atmosphere that is substantially free from water.

[0182] In some embodiments, the preparation of the impure disubstituted beryllium product is performed under an atmosphere optionally selected from nitrogen, argon, or hydrogen.

[0183] In some other embodiments, the preparation of the impure disubstituted beryllium product is performed under a non- inert atmosphere.

[0184] In some embodiments, the preparation of the impure disubstituted beryllium product is performed in a glovebox. In some embodiments, the preparation of the impure disubstituted beryllium product is performed using Schlenk glassware. In some embodiments, the preparation of the impure disubstituted beryllium product is performed using Schlenk glassware in a glovebox. In some embodiments, the preparation of the impure disubstituted beryllium product is performed using Schlenk glassware in a glovebox under an inert atmosphere. In one embodiment, the preparation of the impure disubstituted beryllium product is performed in a nitrogen filled glovebox using a Schlenk flask.

[0185] In some embodiments, the purification of the impure disubstituted beryllium product is performed under an inert atmosphere. In some embodiments, the purification of the impure disubstituted beryllium product is performed under an inert atmosphere that is substantially free from oxygen. In some embodiments, the purification of the impure disubstituted beryllium product is performed under an atmosphere optionally selected from nitrogen, argon, or hydrogen. In some embodiments, the purification of the impure disubstituted beryllium product is performed in a glovebox. In some embodiments, the purification of the impure disubstituted beryllium produce is performed with the aid of Schlenk glassware.

[0186] In one embodiment, the purification of the impure disubstituted beryllium product is performed in a nitrogen filled glovebox. In some embodiments, sublimation of the disubstituted beryllium product is performed under an inert atmosphere. In some embodiments, sublimation of the disubstituted beryllium product is performed under an inert atmosphere that is substantially free from oxygen. In some embodiments, sublimation of the disubstituted beryllium product is performed in a glovebox. In some embodiments, sublimation of the disubstituted beryllium product is performed in a nitrogen- filled glovebox. In some embodiments, sublimation of the disubstituted beryllium product is performed with the aid of Schlenk glassware.

Filtration

[0187] In some embodiments, the solution containing the disubstituted beryllium and the disubstituted beryllium impurity is filtered. In some embodiments, the solution containing the disubstituted beryllium and the disubstituted beryllium impurity is filtered to remove inorganic salts.

[0188] In some embodiments, the filtration is performed with the aid of an adbsorbent, such as Celite, alumina, silica, or charcoal.

Removal of Solvent

[0189] In some embodiments, the solution or reaction mixture containing the disubstituted beryllium product is concentrated to dryness. In some embodiments, the bulk solvent is removed prior to sublimation. In some embodiments, the bulk solvent is removed under reduced pressure prior to sublimation, with the aid of a high performance vacuum line, mechanical pump, or rotary evaporator.

[0190] In some embodiments, the bulk solvent is removed by evaporation at atmospheric pressure.

Disubstituted Beryllium Product

[0191] In some embodiments, the disubstituted beryllium comprises hydrogen, aryl, alkyl, allyl, vinyl, alkenyl, alkynyl, cycloalkyl, heteroaryl, halogen or heterocycloalkyl groups.

[0192] In some embodiments, the disubstituted beryllium is differentially substituted with groups selected from hydrogen, aryl, alkyl, vinyl, alkenyl, allyl, alkynyl, cycloalkyl, heteroaryl,

heterocycloalkyl, or halogen groups.

[0193] In some embodiments, the disubstituted beryllium product is a dialkyl beryllium, such as dimethyl beryllium, diethyl beryllium, dipropyl beryllium, or dibutyl beryllium. In one embodiment, the disubstituted beryllium product is dimethyl beryllium. In one embodiment, the disubstituted beryllium product is diethyl beryllium. In some embodiments, the disubstituted beryllium product is a diaryl beryllium, such as diphenyl beryllium. Methods for making a sublimation vessel that provides uniform heating

[0194] In an aspect of this invention, an apparatus for sublimation is described herein. In a further aspect of this invention, an apparatus for sublimation that provides uniform heating is described herein. [0195] In an aspect of this invention, a sublimation vessel is prepared comprising: a bottom surface and a surrounding wall extending upward from the bottom surface to form a main chamber with one opening; wherein the main chamber houses a heating chamber comprising at least one compartment enclosed by a surrounding wall; wherein the heating chamber is not in communication with the main chamber and has at least one opening for the introduction of heating fluid for heating the main chamber. In one embodiment, a sublimation vessel is produced as illustrated in Figures 1 through 6.

[0196] In some embodiments, the heating chamber is prepared by sealing pieces of glass tubing together. In some embodiments, tubing with an outer diameter ranging from about 1 mm to about 420 mm is used. In one embodiment, tubing with an outer diameter of about 25 mm is used. In some embodiments, tubing with an outer diameter of about 12 to about 15 mm is used. In some embodiments, tubing with lengths ranging from about 1 mm to about 20 cm is used. In some embodiments, the outer diameters of the pieces of tubing are similar or equal to one another. In some embodiments, the outer diameters of the pieces of tubing are not identical to one another. In some embodiments, one piece of tubing has a larger outer diameter than the other pieces of tubing used. In one embodiment, a heating chamber is produced as illustrated in Figure 1.

[0197] In some embodiments, the tubing comprises glass. In some embodiments, the tubing comprises any type of glass that is compatible with the chemicals used. In some embodiments, the tubing comprises any type of glass that is compatible with the temperature used. In some embodiments, the tubing comprises any type of glass that is compatible with the pressure used. In some embodiments, the tubing optionally comprises borosilicate glass; ambered glass; or quartz. In one embodiment, the tubing comprises Type 1, class A, borosilicate glass.

[0198] In some embodiments, a piece of tubing is flattened on one end, referred to herein as the "chimney." In one embodiment, the piece of tubing with the largest outer diameter is used as the chimney. In some embodiments, a piece of glass tubing is sealed to the chimney, and this tube is referred to herein as a "turbo tube." In some embodiments, multiple turbo tubes are used. In one embodiment, the turbo tubes are sealed to the chimney such that they extend out from the chimney in a spoke- like fashion. In some embodiments, the turbo tubes are sealed to the chimney at about a 90 degree angle. In one embodiment, the turbo tubes are separated from one another by approximately 120 degrees. In one embodiment, the turbo tubes are separated from one another by approximately 90 degrees.

[0199] In some embodiments, the sealing is optionally performed manually or using mechanized tools, such as sealing machines and glass blowing lathes.

[0200] In some embodiments, the turbo tubes are sealed to the chimney so that they are flush with the flattened end of the chimney, thereby creating a flattened surface on the top of the heating chamber.

[0201] In some embodiments, the lengths of the turbo tubes are adjusted to fit snugly within the inner diameter of an O-ring flange. In one embodiment, the lengths of the turbo tubes are adjusted to fit within an O-ring flange with an inner diameter of about 50 mm. In some embodiments, the turbo tubes are adjusted to fit snugly within a reaction kettle flange. [0202] In some embodiments, the length of the chimney is adjusted for the amount of material that will be sublimed. In one embodiment, the length of the chimney is about 55 mm from the top of the heating chamber.

[0203] In some embodiments, a reaction kettle flange is used instead of an O-ring flange. In some embodiments, a reaction kettle flange is used with an inner diameter ranging from about 10 mm to about 178 mm. In some embodiments, a reaction kettle flange is used with an inner diameter ranging from about 40 mm to about 60 mm In one embodiment, a reaction kettle flange is used with an inner diameter of about 50 mm.

[0204] In some embodiments, an O-ring flange is used with an inner diameter ranging from about 10 mm to about 178 mm. In some embodiments, an O-ring flange is used with an inner diameter ranging from about 40 mm to about 60 mm. In one embodiment, an O-ring flange is used with an inner diameter of about 50 mm.

[0205] In some embodiments, the chimney is flared such that it fits snugly within the inner diameter of the O-ring flange or O-ring flange stem. In some embodiments, the diameter of the flare for the chimney is slightly smaller than the inner diameter of the O-ring flange or O-ring flange stem. In one

embodiment, the diameter of the chimney flare is about 25 mm.

[0206] In some embodiments, when using a lathe, refractory material is placed between the heat- resistant tube and the glass piece mounted on it. In some embodiments, the refractory material comprises any material that is compatible with the glassblowing process. In some embodiments, the refractory material comprises woven ceramic tapes or woven glass tapes. In some embodiments, refractory material is placed between the heat-resistant tube and the O-ring flange mounted on it. In some embodiments, refractory material is placed between the heat-resistant tube and the heating chamber mounted on it. In some embodiments, the O-ring flange is mounted with chucks on the headstock portion of the lathe. In some embodiments, the heating chamber assembly is mounted with chucks on the tailstock portion of the lathe. In some embodiments, blow hoses are attached to the heat-resistant tubes.

[0207] In some embodiments, the tail stock is traversed so that the heating chamber assembly enters the O-ring flange. In some embodiments, once the flare of the chimney is close to the bottom of the O- ring flange stem, the lathe is rotated and both the bottom of the O-ring flange stem and the outer edge of the flare are heated. In some embodiments, the O-ring flange stem is paddled down until it makes contact with the flare. In some embodiments, heating and blowing is continued until a seal is completed. In one embodiment, a Dewar seal is formed.

[0208] In some embodiments, the turbo tubes are sealed to the O-ring flange stem with the aid of a lathe. In some embodiments the turbo tubes are sealed manually. In some embodiments, the sublimation vessel is annealed in an annealing oven.

[0209] In some embodiments, the collection plate comprises any material that is compatible with the temperature, pressure, and chemicals used in the sublimation. In some embodiments, the collection plate comprises a porous material, e.g., a frit. In some embodiments, the collection plate comprises a nonporous material. In some embodiments, the collection plate comprises glass. In one embodiment, the collection plate comprises a metal.

EXAMPLES

[0210] The present invention may be better understood through reference to the following examples. These examples are included to describe exemplary embodiments only and should not be interpreted to encompass the entire breadth of the invention.

Example 1- Preparation of 95% Pure Dimethyl Beryllium

[0211] In a nitrogen filled glovebox, a 500 mL Schlenk flask is charged with BeCi ₂ (15 g, 188 mmol). The BeCi ₂ is dissolved in cold (-30 °C) and dry diethyl ether (125 mL), which results in the formation of a turbid solution. To this solution, 128.25 mL of MeMgBr (3 M in diethyl ether, 386 mmol) is added in a dropwise manner. The resulting cloudy suspension is stirred in the glovebox for 16 hours and then is filtered over dry Celite to remove precipitated magnesium salts. The ethereal solution is concentrated to dryness on a high performance vacuum line. The obtained solid residue is transferred into the custom sublimation vessel, with an attached condenser, wherein it is heated slowly from ambient temperature to 150 °C under high dynamic vacuum When the oil bath temperature reaches about 85 °C, the product begins to sublime. The sublimation is repeated multiple times to afford pure BeMe ₂ . ^ι ΐΙ NMR analysis indicates that the BeMe ₂ is greater than or equal to 95% pure.

Example 2- Preparation of Dimethyl Beryllium using a Normal Sublimation Vessel

[0212] In a nitrogen filled glovebox, a 500 mL Schlenk flask is charged with BeCi ₂ (15 g, 188 mmol). The BeCi ₂ is dissolved in cold (-30 °C) and dry diethyl ether (125 mL), which results in the formation of a turbid solution. To this solution, 128.25 mL of MeMgBr (3 M in diethyl ether, 386 mmol) is added in a dropwise manner. The resulting cloudy suspension is stirred in the glovebox for 16 hours and then is filtered over dry Celite to remove precipitated magnesium salts. The ethereal solution is concentrated to dryness on a high performance vacuum line. The obtained solid residue is transferred into a normal sublimation vessel, with an attached condenser, wherein the dimethyl beryllium is sublimed multiple times. This procedure is repeated multiple times and dimethyl beryllium that is contaminated with dimethyl beryllium diethyl etherate is consistently obtained. ^l H NMR analysis of several different batches of sublimed product shows that about 2.0 to about 0.5 molecules of diethyl ether are coordinated to every molecule of dimethyl beryllium.

Example 3- Method for Making the Sublimation Vessel

[0213] The heating chamber portion of the sublimation vessel is created by sealing four pieces of tubing together. First, a piece of tubing with an outer diameter of about 25 mm is flattened on one end to create a "chimney", and then three pieces of tubing ("turbo tubes") with outer diameters of about 12 mm are connected to the chimney via a side-seal at about a 90 degree angle. The turbo tubes extend from the chimney in a spoke-like arrangement. The turbo tubes are sealed to the chimney so that they are flush with the flattened end of the chimney, thereby creating a flattened surface on the top of the heating chamber. The three pieces of tubing are separated from one another by approximately 120 degrees. The turbo tubes are cut and beaded so that they fit just within the inner diameter of an O-ring flange with a 50 mm inner diameter. The chimney is cut 55 mm from its top and flared so that the outer edge of the flare fits snugly within the O-ring flange stem. The flare is started at about 30 mm down from the top of the chimney. Refractory material is placed between the heating chamber and the heat-resistant hollow tube on which it is mounted.

[0214] A commercially-available O-ring flange with about a 50 mm inner diameter and a glass stem with a length of about 11 cm is mounted with chucks on the headstock portion of the lathe. The heating chamber assembly is mounted with chucks on the tailstock portion of the lathe. Blow hoses are attached to the heat-resistant tubes. The tail stock is traversed until the chimney flare of the heating chamber assembly is close to the bottom of the O-ring flange stem. The lathe is rotated and the bottom of the O- ring flange stem and the outer edge of flare are heated. The O-ring flange stem is paddled down until it makes contact with the flare. Heating and blowing are continued until a Dewar seal is completed. The turbo tubes are sealed to the O-ring flange stem using the following sequence of steps: (1) the area where the turbo tube contacts the O-ring flange stem is heated and the turbo tubes are sealed to the wall of the stem; (2) a bubble is blown out in the tube without opening the bubble and without affecting the flattened area of the ring seal; (3) steps 1 and 2 are performed on the remaining two tubes; and (4) the bubbles of all three turbo tubes are then picked and blown open. Finally, the temperature of the sublimation vessel is stabilized. It is removed from the lathe and placed into an annealing oven that is preheated to 375 °C. The temperature of the annealing oven is increased to 565 °C and the sublimation vessel is removed once it is sufficiently annealed.

[0215] Overall, these results demonstrate that substantially pure disubstituted beryllium can be prepared. In addition, these results demonstrate that a sublimation vessel can be prepared that comprises a heating chamber that provides uniform heating.

[0216] While preferred embodiments of the present invention have been shown and described herein, it will be obvious to those skilled in the art that such embodiments are provided by way of example only. Numerous variations, changes, and substitutions will now occur to those skilled in the art without departing from the invention. It should be understood that various alternatives to the embodiments of the invention described herein may be employed in practicing the invention. It is intended that the following claims define the scope of the invention and that methods and structures within the scope of these claims and their equivalents be covered thereby.