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Title:
PROCESS FOR THE PREPARATION OF STEROIDAL CARBOTHIOIC ACID DERIVATIVES AND INTERMEDIATES
Document Type and Number:
WIPO Patent Application WO/2004/087731
Kind Code:
A1
Abstract:
A method for the conversion of steroidal 17β-carboxylic acids to c carbothioic acid and esters thereof such as fluticasone propionate.

Inventors:
Loevli, Trond (Welhavens Vei 2, Sofiemyr, NO-1412, NO)
Nygaard, Anne-mette (Harald Haarfagres Gates 10B, Oslo, NO-0363, NO)
Reitstoen, Bjoern (Ekelyveien 4B, Oslo, NO-0374, NO)
Fivelstad, Magny (Sognsveien 131B, Oslo, NO-0855, NO)
Application Number:
PCT/DK2004/000242
Publication Date:
October 14, 2004
Filing Date:
April 02, 2004
Export Citation:
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Assignee:
Alpharma, Aps (11 Dalslandsgade, Copenhagen S, DK-2300, DK)
Loevli, Trond (Welhavens Vei 2, Sofiemyr, NO-1412, NO)
Nygaard, Anne-mette (Harald Haarfagres Gates 10B, Oslo, NO-0363, NO)
Reitstoen, Bjoern (Ekelyveien 4B, Oslo, NO-0374, NO)
Fivelstad, Magny (Sognsveien 131B, Oslo, NO-0855, NO)
International Classes:
C07J3/00; C07J31/00; C07J; (IPC1-7): C07J3/00; C07J31/00
Domestic Patent References:
WO1997024365A11997-07-10
WO2002008243A12002-01-31
WO2002012265A12002-02-14
Foreign References:
GB2088877A1982-06-16
US4578221A1986-03-25
Other References:
HAPGOOD, JANET P. ET AL: "Steroid-affinity purification of the rat liver glucocorticoid hormone receptor complex", JOURNAL OF STEROID BIOCHEMISTRY ( 1987 ), 28(6), 769-77 CODEN: JSTBBK; ISSN: 0022-4731, 1987, XP001183044
HOYTE, R. M. ET AL: "Synthesis and evaluation of potential radioligands for the progesterone receptor", JOURNAL OF MEDICINAL CHEMISTRY ( 1985 ), 28(11), 1695-9 CODEN: JMCMAR; ISSN: 0022-2623, 1985, XP001182782
MACINDOE, JOHN H. ET AL: "Comparative studies of 5.alpha.-reductase inhibitors within MCF-7 human breast cancer cells", JOURNAL OF STEROID BIOCHEMISTRY ( 1984 ), 20(5), 1095-100 CODEN: JSTBBK; ISSN: 0022-4731, 1984, XP001182781
FORMSTECHER, P. ET AL: "Synthesis of steroidal 17.beta.-carboxamide derivatives", STEROIDS ( 1980 ), 35(3), 265-72 CODEN: STEDAM; ISSN: 0039-128X, 1980, XP001182780
KOLBE, ADELHEID ET AL: "Syntheses of dexamethasone conjugates of the phytohormones gibberellin A3 and 24-epicastasterone", COLLECTION OF CZECHOSLOVAK CHEMICAL COMMUNICATIONS ( 2002 ), 67(1), 103-114 CODEN: CCCCAK; ISSN: 0010-0765, 2002, XP001194682
HEUBNER, ARNULF ET AL: "Application of liquid-liquid partition chromatography in the simultaneous purification of sex-hormone-binding globulin and corticosteroid-binding globulin", JOURNAL OF CHROMATOGRAPHY ( 1987 ), 397, 419-34 CODEN: JOCRAM; ISSN: 0021-9673, 1987, XP001194688
PHILLIPPS G H ET AL: "SYNTHESIS AND STRUCTURE-ACTIVITY RELATIONSHIPS IN A SERIES OF ANTIINFLAMMATORY CORTICOSTEROID ANALOGUES, HALOMETHYL ANDROSTANE- 17BETA-CARBOTHIOATES AND-17BETA-CARBOSELENOATES", JOURNAL OF MEDICINAL CHEMISTRY, AMERICAN CHEMICAL SOCIETY. WASHINGTON, US, vol. 37, no. 22, 1 October 1994 (1994-10-01), pages 3717 - 3729, XP002025925, ISSN: 0022-2623
MANZ, BERNHARD ET AL: "Synthesis of biotin-labeled dexamethasone derivatives. Novel hormone-affinity probes", EUROPEAN JOURNAL OF BIOCHEMISTRY ( 1983 ), 131(2), 333-8 CODEN: EJBCAI; ISSN: 0014-2956, 1983, XP009034828
GOVINDAN, MANJAPRA V. ET AL: "Three-step purification of glucocorticoid receptors from rat liver", EUROPEAN JOURNAL OF BIOCHEMISTRY ( 1980 ), 108(1), 47-54 CODEN: EJBCAI; ISSN: 0014-2956, 1980, XP009034821
Attorney, Agent or Firm:
Lawrence, Malcolm Graham (HLBBshaw, Merlin House Falconry Court, Baker's Lan, Epping Essex CM16 5DQ, GB)
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Claims:
CLAIMS
1. Device for heating an object, in particular a wafer of semiconductor material, comprising: a chamber in which the object for heating can be placed and which is provided with a wall permeable to radia tion in a determined wavelength range, heating elements for heating the object in the chamber, first radiating elements for projecting radiation onto the object, means for modulating the intensity of the radiation coming from the first radiating elements, a radiation meter for measuring the radiation intensity generated by the object, the sensitivity of which is located for a significant part in said wavelength range, and filtering means for filtering in said wavelength range radiation coming from the heating means and/or parts heated by the heating means, wherein the filtering means are disposed such that radiation from the modulated first radia ting elements reaches the radiation meter unfiltered.
2. Device as claimed in claim 1, wherein the heating elements comprise second radiating elements.
3. Device as claimed in claim 1 or 2, wherein the heating elements comprise a reflecting wall.
4. Device as claimed in claim 1, 2 or 3, wherein the determined wavelength range is situated round 15 μm, in preference round 2.95 μm.
5. Device as claimed in claim 4, wherein the filtering means contain PyrexR or Robax".
6. Method for heating an object using heating elements, wherein the temperature of the object is measured using modulated radiation which is projected onto the object in a wavelength range in which no radiation is projected onto the object by the heating elements.
7. Device provided for heating an object, in particular a wafer of semiconductor material, comprising: a chamber in which the object for heating can be placed and which is provided with a wall permeable to radia tion in a determined wavelength range, heating elements for heating the object in the chamber, radiating elements for projecting radiation to compensate for variations in the reflectivity and/or emissivity of the object, a radiation meter for measuring the radiation intensity generated by the object, the sensitivity of which is located for a significant part in said wavelength range, and filtering means for filtering in said wavelength range radiation coming from the heating means and/or parts heated by the heating means, wherein the filtering means are disposed such that radiation from the compensating radiating elements reaches the radiation meter unfiltered.
8. Device as claimed in claim 1 or 7, wherein the radiation meter extends beyond the filtering means in the direction of the object.
9. Use of device as claimed in any of the claims 15, 7 and/or 8, wherein the object is heated to a temperature of approximately 250500°C or 4501000°C.
Description:
DEVICE AND METHOD FOR HEATING OBJECTS WHEREIN THE TEMPERATURE OF THE OBJECT IS MEASURED

In the heating of wafers of semiconductor material use is frequently made of halogen lamps or arc lamps as heating elements. For accurate heating of these objects to a determined temperature a large scale search is in progress for an accurate, non-contact temperature measurement - see for instance the American patent specification 4.919.542 and the German Offenlegungsschrift 4012615. Pyrometers applied in such temperature measurements are susceptible to disturbances due to radiation coming from the lamp, while these measurements are also dependent on the emissivity of the object.

An earlier proposal, PCT/EP92/00039, the content of which can be deemed as interpolated herein, relates to the modulating of heating lamps. Modulation of the heating lamps reduces the effectiveness of the heating of the object. In addition the temperature measurement is disturbed by the lamps because of the changing intensity thereof.

A first aspect of the present invention provides a device for heating an object, in particular a wafer of semi- conductor material, comprising:

- a chamber in which the object for heating is to be placed and which is at least partially provided with a wall permeable to radiation in a determined wavelength range, - heating elements for heating the object in the chamber,

- first radiating elements for projecting radiation onto the object,

- means for modulating the intensity of the radiation coming from the first radiating elements,

- a radiation meter for measuring the radiation intensity generated by the object, the sensitivity of which is considerable in at least said wavelength range, and

- filtering means for filtering in said wavelength range radiation coming from the heating means and/or parts heated by the heating means, wherein the filtering means are disposed such that the radiation coming from the modulated first radiating elements reaches the radiation meter unfil- tered.

Using the first radiating elements, which also perhaps contribute partially to the heating of the object, the emissivity of the object can be determined accurately. It has been found in practice that modulation of the lamps is particularly suitable for heating objects in a temperature range of approximately 450-1000°C.

According to a further aspect of the present application a device is provided for heating an object, in particular a wafer of semiconductor material, comprising:

- a chamber in which the object for heating can be placed and which is provided with a wall permeable to radia¬ tion in a determined wavelength range,

- heating elements for heating the object in the chamber,

- radiating elements for projecting radiation to compensate for variations in the reflectivity and/or emissivity of the object,

- a radiation meter for measuring the radiation intensity generated by the object, the sensitivity of which is located for a significant part in said wavelength range, and

- filtering means for filtering in said wavelength range radiation coming from the heating means and/or parts heated by the heating means, wherein the filtering means are disposed such that radiation from the compensating radiating elements reaches the radiation meter unfiltered.

Such a device is particularly advantageous in the temperature range of 250-500°C.

Further advantages, features and details of the present invention will become apparent in the light of a description of the preferred embodiment thereof with reference to the annexed drawing, in which: fig. 1 shows a diagram of a first preferred embodiment of the device according to the present invention; fig. 2 shows a diagram of a second preferred embodiment of the present invention; fig. 3 shows a diagram of a third preferred embodiment of the present invention; and fig. 4 shows a diagram of a fourth preferred embodiment of the present invention.

A device 1 (fig. 1) comprises a chamber 2, for instance of quartz, in which is placed an object W, in the present case a wafer of semiconductor material. Heating elements 3, preferably halogen lamps, serve to heat the wafer of semiconductor material . Arranged between lamps 3 and wafer W is a filter 4 which is impermeable to determined wavelengths to which the chamber 2 is permeable. Radiating elements 5, preferably halogen lamps, are disposed between filter 4 and chamber 2. Arranged for measuring the radiation from the wafer is a pyrometer 6, the light access of which extends through the filter 4. The pyrometer 6 is coupled to a control member 7 for controlling the lamps 3 and lamps 5. The intensity of the lamps 5 is modulated with a determined amount of modulation depth. In order to measure the modula¬ ted radiation coming directly from the lamps 5 a further pyrometer 8 is arranged in the present embodiment. Pyrometer 6 is substantially sensitive to radiation of that wavelength to which the filter 4 is impermeable. The measurement of the reflectivity, and therefore the emissivity, of the object is therefore not disturbed by the heating lamps 3. The chamber 2 can consist of a simple quartz tube without modifications thereto being necessary.

Use of a plate of Pyrex" glass with a thickness of 8 mm provides a considerable filtering action in a region round a wavelength of 2.95 μm, to which wavelength quartz and therefore the chamber 2 is permeable. If a plate of Robax R of 5 mm thickness is chosen for the filter 4 a sufficient filtering action round 2.95 μm is also obtained.

In a second embodiment heating lamps 3 , 3 ' are disposed on both sides of chamber 2, filters 4, 4 1 likewise on both sides in addition to modulated halogen lamps 5, 5' on both sides. In the arrangement according to fig. 2 a uniform heating of wafer W is obtained, while an accurate temperature measurement is ensured. To heat a wafer of semiconductor material on both sides (fig. 3) a reflecting wall 9 can also be placed opposite the lamps 3, 5. In an embodiment wherein an object S is as good as impermeable to the heating radiation, for instance a steel plate, schematically designated heating elements 11 can be disposed on one side, while modulated lamps 5 are disposed on the opposite side. The filter 4 is in this case included to filter background radiation from a wall 10 out of the radiation reflected by the plate S.

It has been found in practical tests that lamps compensating for emissivity and/or reflection of the object, as described in EP-A-91201121.0 in particular for heating the object in a temperature range of 250-500°C can likewise be advantageously employed in a device wherein the heating lamps are disposed in relation to the chamber behind the filtering means and wherein the compensating lamps are dis¬ posed between the filtering means and the chamber, while the radiation meter extends through the filtering means towards the object. In the above mentioned publication of the same inventor and applicant a filter is described in the form of two filter plates with water therebetween.

Further modifications of the device and method according to the present invention are conceivable; for instance:

- if the object consists of a forward moving belt or an object being moved forward, the reflectivity (and the emissivity) thereof can be determined using a first measurement according to the present invention, while in further process steps the object temperature can be determined from direct measurements in correlation with the first measurement.

- using one or more mirrors the modulated radiation in the arrangement can be reflected without the modulated radiation sources having to be disposed in the arrangement.