LANEMAN SCOTT A (US)
US20120308739A1 | 2012-12-06 | |||
US20020032288A1 | 2002-03-14 | |||
US20060068103A1 | 2006-03-30 | |||
US20180087164A1 | 2018-03-29 |
What is claimed is: 1. A process for preparing a compound of the Formula (I): wherein R and R1 are independently chosen from hydrogen and C1-C8 alkyl; the process comprising: contacting a compound of the formula with WCl6; and adding a hydride reagent. 2. The process of claim 1, wherein the hydride reagent is NaBH4, LiAlH4, LiBH4, LiBH(CH3CH2)3, [(isobutyl)2AlBH4], NaBH3CN, Na[HB(OC(O)CH3)], BH3- tetrahydrofuran, BH3-S(CH3)2, diisobutylaluminum hydride, or sodium bis(2- methoxyethoxy)aluminium hydride. 3. The process of claim 1 or 2, wherein R and R1 is hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, n-pentyl, isopentyl, sec-pentyl, n-hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec-heptyl, n-octyl, isooctyl, or sec-octyl. 4. The process of any preceding claim, wherein R and R1 are methyl. 5. The process of any preceding claim, wherein the hydride reagent is NaBH4. 6. The process of any preceding claim, wherein the hydride reagent is NaBH4 and each of R and R1 are methyl. 7. The process of any preceding claim, wherein the compound of Formula (I) has less than about 0.5 weight percent of multi-alkylated species. 8. The process of any preceding claim, wherein the compound of Formula (I) is devoid of dicyclopentadiene and mixed cyclopentadiene species. 9. A compound comprising Formula (I): ( ), wherein R and R1 are independently chosen from hydrogen and C1-C8 alkyl, and wherein the compound of Formula (I) has less than about 0.5 weight percent of multi- alkylated species, as determined by gas chromatography. 10. The compound of claim 9, wherein the compound of Formula (I) is further devoid of dicyclopentadiene and mixed dicyclopentadiene species. 11. A process for preparing a compound of the Formula (I): wherein R and R1 are independently chosen from hydrogen and C1-C8 alkyl, the process comprising: contacting a compound of the formula with a dialkyl magnesium compound to provide a compound of the formula adding WCl6; and adding a hydride reagent. 12. The process of claim 11, wherein the hydride reagent is NaBH4, LiAlH4, LiBH4, LiBH(CH3CH2)3, [(isobutyl)2AlBH4], NaBH3CN, Na[HB(OC(O)CH3)], BH3- tetrahydrofuran, BH3-S(CH3)2, diisobutylaluminum hydride, or sodium bis(2- methoxyethoxy)aluminium hydride. 13. The process of claim 11 or 12, wherein the hydride reagent is NaBH4. 14. The process of any of claims 11 to 13, wherein R and R1 are hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, n-pentyl, isopentyl, sec-pentyl, n- hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec-heptyl, n-octyl, isooctyl, or sec- octyl. 15. The process of any of claims 11 to 14, wherein R and R1 are methyl. 16. The process of any of claims 11 to 15, wherein the hydride reagent is NaBH4. 17. The process of any of claims 11 to 16, wherein the hydride reagent is NaBH4 and each of R and R1 are methyl. 18. The process of any of claims 11 to 17, wherein the dialkyl magnesium compound is a di(C1-C8 alkyl)magnesium compound. 19. The process of any of claims 11 to 17, wherein the dialkyl magnesium compound is Mg(CH2CH2CH2CH3)2 or Mg[(CH)(CH3)(CH2CH3)][CH2CH2CH2CH3]. 20. A process for preparing a compound of the Formula (II): wherein M is chosen from Hf, Zr, Ti, Ta, Nb, W, and Mo, and wherein R and R1 are independently chosen from hydrogen and C1-C8 alkyl, the process comprising: contacting a compound of the formula with a compound of the formula MX4, wherein X is chloro, bromo, or iodo. 21. The process of claim 20, wherein M is Hf, Zr, Ti, W, or Mo. 22. The process of claim 20 or 21, wherein R and R1 are hydrogen, methyl, ethyl, n- propyl, isopropyl, n-butyl, isobutyl, sec-butyl, n-pentyl, isopentyl, sec-pentyl, n-hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec-heptyl, n-octyl, isooctyl, or sec-octyl. 23. The process of any of claims 20 to 22, wherein R and R1 are methyl. 24. A compound comprising Formula (II): ( ), wherein M is Hf, Zr, Ti, Ta, Nb, W, or Mo, wherein X is chloro, bromo, or iodo, and wherein the compound of Formula (III) has less than about 0.5 weight percent of multi-alkylated species, as determined by gas chromatography. 25. The compound of claim 24, wherein M is Hf, Zr, Ti, W, or Mo. 26. The compound of claim 24 or 25, wherein the compound of Formula (III) is further devoid of dicyclopentadiene and mixed dicyclopentadiene species. |
with WCl 6 and adding a hydride reagent. [0026] In a second aspect, the disclosure provides the process of the first aspect, wherein the hydride reagent is NaBH 4 , LiAlH 4 , LiBH 4 , LiBH(CH 3 CH 2 ) 3 , [(isobutyl) 2 AlBH 4 ], NaBH 3 CN, Na[HB(OC(O)CH 3 )], BH 3 -tetrahydrofuran, BH 3 -S(CH 3 ) 2 , diisobutylaluminum hydride, or sodium bis(2-methoxyethoxy)aluminium hydride. [0027] In a third aspect, the disclosure provides the process of the first or second aspect, wherein R and R 1 are hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec- butyl, n-pentyl, isopentyl, sec-pentyl, n-hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec- heptyl, n-octyl, isooctyl, or sec-octyl. [0028] In a fourth aspect, the disclosure provides the process of the first, second, or third aspect, wherein R and R 1 are methyl. [0029] In a fifth aspect, the disclosure provides the process of any one of the first through the fourth aspects, wherein the hydride reagent is NaBH 4 . [0030] In a sixth aspect, the disclosure provides the process of any one of the first through the fifth aspects, wherein the compound of Formula (I) has less than about 0.5 weight percent, less than about 0.3 weight percent, or less than about 0.1 weight percent of multi- alkylated species. [0031] In a seventh aspect, the disclosure provides the process of any one of the first through the eighth aspects, wherein the compound of Formula (I) is devoid of dicyclopentadiene and mixed cyclopentadiene species. [0032] In an eighth aspect, the disclosure provides a compound of the Formula (I):
wherein R and R 1 are independently chosen from hydrogen and C 1 -C 8 alkyl, and wherein the compound of Formula (I) has less than about 0.5 weight percent of multi- alkylated species, as determined by gas chromatography. [0033] In a ninth aspect, the disclosure provides the compound of the eighth aspect, wherein the compound of Formula (I) has less than about 0.3 weight percent or less than about 0.1 weight percent of multi-alkylated species, as determined by gas chromatography. [0034] In a tenth aspect, the disclosure provides the compound of the ninth or tenth aspect, wherein the compound of Formula (I) is further devoid of dicyclopentadiene and mixed dicyclopentadiene species. [0035] In an eleventh aspect, the disclosure provides a process for preparing a compound of the Formula (I): wherein R and R 1 are independently chosen from hydrogen and C 1 -C 8 alkyl; which comprises contacting a compound of the formula with a dialkyl magnesium compound to provide a compound of the formula Adding WCl6, and adding a hydride reagent. [0036] In a twelfth aspect, the disclosure provides the process of the eleventh aspect, wherein the hydride reagent is NaBH 4 , LiAlH 4 , LiBH4, LiBH(CH 3 CH 2 ) 3 , [(isobutyl) 2 AlBH 4 ], NaBH 3 CN, Na[HB(OC(O)CH 3 )], BH 3 -tetrahydrofuran, BH 3 -S(CH 3 ) 2 , diisobutylaluminum hydride, or sodium bis(2-methoxyethoxy)aluminum hydride. [0037] In a thirteenth aspect, the disclosure provides the process of the eleventh or twelfth aspect, wherein the hydride reagent is NaBH 4 . [0038] In a fourteenth aspect, the disclosure provides the process of the process of any one of the eleventh through thirteenth aspects, wherein R and R 1 are hydrogen, methyl, ethyl, n- propyl, isopropyl, n-butyl, isobutyl, sec-butyl, n-pentyl, isopentyl, sec-pentyl, n-hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec-heptyl, n-octyl, isooctyl, or sec-octyl. [0039] In a fifteenth aspect, the disclosure provides the process of any one of the eleventh through fourteenth aspects, wherein R and R 1 are methyl. [0040] In a sixteenth aspect, the disclosure provides the process of any one of the eleventh through fifteenth aspects, wherein the hydride reagent is NaBH4. [0041] In a seventeenth aspect, the disclosure provides the process of any one of the eleventh through the sixteenth aspects, wherein the dialkyl magnesium compound is Mg(C2-C8 alkyl)2, Mg(C3-C8 alkyl)2, or Mg(C4-C8 alkyl)2. [0042] In an eighteenth aspect, the disclosure provides the process of any one of the eleventh through the seventeenth aspects, wherein the dialkyl magnesium compound is Mg(CH2CH2CH2CH3)2 or Mg[(CH)(CH3)(CH2CH3)][CH2CH2CH2CH3]. [0043] In a nineteenth aspect, the disclosure provides a process for preparing a compound of the Formula (II) ( ), wherein M is chosen from Hf, Zr, Ti, Ta, Nb, W, and Mo; wherein R and R 1 are independently chosen from hydrogen and C1-C8 alkyl; which comprises contacting a compound of the formula
with a compound of the formula MX 4 , wherein X is chloro, bromo, or iodo. [0044] In a twentieth aspect, the disclosure provides the process of the nineteenth aspect, wherein M is Hf, Zr, Ti, W, or Mo. [0045] In a twenty-first aspect, the disclosure provides the process of the nineteenth or twentieth aspect, wherein R and R 1 are hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, n-pentyl, isopentyl, sec-pentyl, n-hexyl, isohexyl, sec-hexyl, n-heptyl, isoheptyl, sec-heptyl, n-octyl, isooctyl, or sec-octyl. [0046] In a twenty-second aspect, the disclosure provides the process of the nineteenth, twentieth, or twenty-first aspect, wherein R and R 1 are methyl. [0047] In a twenty-third aspect, the disclosure provides a compound of the Formula (II):
wherein M is Hf, Zr, Ti, Ta, Nb, W, or Mo; and X is chloro, bromo, or iodo; and wherein the compound of Formula (III) has less than about 0.5 weight percent of multi-alkylated species, as determined by gas chromatography. [0048] In a twenty-fourth aspect, the disclosure provides the compound of the twenty-third aspect, wherein M is Hf, Zr, Ti, W, or Mo. [0049] In a twenty-fifth aspect, the disclosure provides the compound of the twenty-third or twenty-fourth aspect, wherein the compound of Formula (III) has less than about 0.3 weight percent or less than about 0.1 weight percent of multi-alkylated species. [0050] In a twenty-sixth aspect, the disclosure provides the compound of the twenty-third, twenty-fourth, or twenty-fifth aspects, wherein the compound of Formula (III) is further devoid of dicyclopentadiene and mixed dicyclopentadiene species. [0051] Having thus described several illustrative embodiments of the present disclosure, those of skill in the art will readily appreciate that yet other embodiments may be made and used within the scope of the claims hereto attached. Numerous advantages of the disclosure covered by this document have been set forth in the foregoing description. It will be understood, however, that this disclosure is, in many respects, only illustrative. The disclosure’s scope is, of course, defined in the language in which the appended claims are expressed.
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