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1. 发明申请

US20220064099A1 Method for Making a Di(aminoaryl)fluorene compound 有权
公开(公告)号：US20220064099A1
公开(公告)日：2022-03-03
申请号：US17415378
申请日：2019-12-20
申请人： Cytec Industries Inc.
发明人： Jonathan E. MEEGAN , Victor MARUANI , Vincent SCHANEN , Paul CROSS
IPC分类号： C07C209/84
摘要： The present invention is directed to a method for making a di(aminoaryl)fluorene compound that includes the steps of: (a) reacting a fluorenone compound according structure (I) with excess aminobenzene according to structure (II) wherein: each R1, R2, R3, R4, R12, and R13 is independently a group that is inert in the polymerization each R1, of epoxy compounds, and R11 is H or (C1-C6)alkyl, in the presence of an acid catalyst, in a liquid medium comprising an aromatic or substituted aromatic solvent having a boiling point of greater than or equal to 150° C. and in the presence of an acid catalyst, in a liquid medium comprising an aromatic or substituted aromatic solvent having a boiling point of greater than or equal to 150° C. and from which the di(aminoaryl)fluorene compound is crystallizable, to form a crude product mixture comprising the di(aminoaryl)fluorene compound, (b) crystallizing di(aminoaryl)fluorene compound in the product mixture, and (c) separating the product mixture into crystallized di(aminoaryl)fluorene compound and a filtrate.

2. 发明申请

US20210371372A1 METHOD FOR THE PRODUCTION OF ETHYLENEAMINES 有权
公开(公告)号：US20210371372A1
公开(公告)日：2021-12-02
申请号：US16759428
申请日：2018-10-17
申请人： BASF SE
发明人： Hermann LUYKEN
IPC分类号： C07C209/84
摘要： The present invention relates to a process for purifying ethylenediamine, in which a) a mixture comprising water (H2O), ethylenediamine (EDA) and N-methylethylenediamine (NMEDA) is introduced into a rectification column (NMEDA removal column), where the mixture introduced comprises at least the amount of water as required for the formation of a high-boiling azeotrope of EDA and water at the appropriate bottom temperature; and the EDA-comprising bottom product from the NMEDA removal column is introduced into a second rectification column (EDA dewatering column), wherein the pressure at the top of the EDA dewatering column is adjusted such that the boiling temperature of the mixture obtained at the top is 10° C. or higher than the bottom temperature of the NMEDA removal column, which comprises (i) partly or fully condensing the vapors from the top of the EDA dewatering column in a condenser which is cooled with a medium which is at least partly evaporated during the condensation and the vapor thus formed is used at least partly to heat the evaporator of the NMEDA removal column; and/or (ii) introducing the vapors from the top of the EDA dewatering column into the NMEDA removal column.

3. 发明授权

US10947184B2 Crystalline form of triethylenetetramine tetrahydrochloride and its pharmaceutical use 有权
公开(公告)号：US10947184B2
公开(公告)日：2021-03-16
申请号：US16917266
申请日：2020-06-30
申请人： ORPHALAN S.A.
发明人： Timothy James Morley , Ronnie Maxwell Lawrence , Naseem Amin
IPC分类号： C07C211/14 , C07C209/84 , A61K9/00
摘要： The present invention describes a new crystalline form of triethylenetetramine tetrachloride which has improved room temperature stability over known forms and over the dichloride salt. The new crystalline form is characterised by having peaks in an XRPD spectrum at 22.9, 25.4, 25.8, 26.6, 34.6 and 35.3±0.1°2θ and Raman shifts 943, 1173, 1527 and 1612±5 cm−1. The crystalline form of triethylenetetramine tetrachloride is useful in the treatment of Wilson's disease.

4. 发明授权

US10889539B2 Aniline purification process 有权
公开(公告)号：US10889539B2
公开(公告)日：2021-01-12
申请号：US16654303
申请日：2019-10-16
申请人： COVESTRO DEUTSCHLAND AG
发明人： Michael Merkel , Friedhelm Steffens , Murat Kalem , Peter Lehner
IPC分类号： C07C209/84 , B01D3/14 , B01D3/36 , B01D5/00 , C07C211/46
摘要： The present invention concerns a process for the preparation of pure aniline, comprising the steps of a) providing a crude aniline fraction containing up to 20.000% by weight of phenol; b) dividing the crude aniline fraction from step a) into a first partial stream and a second partial stream; c) distilling the first partial stream from step b) in a first distillation column and distilling the second partial stream from step b) in a second distillation column, wherein the first distillation column is operated at a higher head pressure than the second distillation column, with the proviso that each of the first distillation column and the second distillation column is operated at a head pressure in the range from 1.0 mbar(abs.) to 500 mbar(abs.), and wherein from each of the first distillation column and the second distillation column, (i) a gaseous aniline distillate (=purified aniline) is removed as the overhead product and subsequently condensed, wherein a first partial stream of the condensed aniline distillate is returned to the first and/or the second distillation column as a reflux stream and a second partial stream of the condensed aniline distillate is removed as the product stream, and (ii) a liquid bottom stream which is concentrated in phenol is removed, from which a first portion is partially or completely vaporised and is returned to the respective distillation column, and from which a second portion is discharged; d) using the heat released during the condensation of the aniline distillate from the first distillation column in order to provide the heat necessary for vaporising the first portion of the bottom stream from the second distillation column.

5. 发明授权

US10456749B2 System for the removal of heat stable amine salts from an amine absorbent 有权
公开(公告)号：US10456749B2
公开(公告)日：2019-10-29
申请号：US15253243
申请日：2016-08-31
申请人： General Electric Technology GmbH , DOW GLOBAL TECHNOLOGIES LLC
发明人： Nareshkumar B. Handagama , Barath Baburao , Frederic Vitse , Stephen A. Bedell , Jonathan W. Leister , Ross Dugas
IPC分类号： B01D53/14 , B01D61/42 , B01J47/00 , C07C209/84
摘要： A system for the removal of heat stable amine salts from an amine absorbent used in a carbon dioxide (CO2) capture process.

6. 发明申请

US20190233366A1 CRYSTALLINE DIETHYLAMINE TETRATHIOMOLYBDATE AND ITS PHARMACEUTICAL USES 审中-公开
公开(公告)号：US20190233366A1
公开(公告)日：2019-08-01
申请号：US16340939
申请日：2017-10-20
申请人： UCL BUSINESS PLC.
发明人： Alex Peter DYSON , Daniel GOODING , Joanne HOLLAND
IPC分类号： C07C211/05 , C07C209/84 , A61P9/10
摘要： The invention relates to a crystalline diethylamine tetrathiomolybdate salt (DEA-TTM). The invention also relates to methods for producing the crystalline DEA-TTM salt of the invention. The invention also relates to pharmaceutical compositions comprising the crystalline DEA-TTM salt of the invention. The invention also relates to the use of the crystalline DEA-TTM salt of the invention in the treatment of the human or animal body, in particular its use in treatment of a condition requiring reduced metabolism of an organ or the whole body of a patient, by administering to a patient in need thereof a therapeutically effective amount of the crystalline DEA-TTM salt.

7. 发明授权

US10351509B2 Fenfluramine compositions and methods of preparing the same 有权
公开(公告)号：US10351509B2
公开(公告)日：2019-07-16
申请号：US15385525
申请日：2016-12-20
申请人： ZOGENIX INTERNATIONAL LIMITED
发明人： Derek J. Londesbrough , Marc W. Andersen
IPC分类号： C07C209/28 , C07C51/43 , C07C51/08 , C07C45/80 , C07C45/72 , C07C209/84
摘要： Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and(c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.

8. 发明授权

US10069070B2 Method and apparatus for purifying organic material by using ionic liquid 有权
公开(公告)号：US10069070B2
公开(公告)日：2018-09-04
申请号：US15118288
申请日：2015-02-11
申请人： ILSOLED CO., LTD.
发明人： Tae Won Kim
IPC分类号： H01L51/00 , H01L51/56 , B01D7/00 , B01D9/00 , C07C209/84 , C07C211/54 , H01L51/50
摘要： A method of purifying an organic material using an ionic liquid according to the present invention includes a sublimation step (S510) of sublimating the organic material containing an impurity, a capturing step (S520) of bringing a sublimated gas of the organic material into contact with the flowing ionic liquid to capture the sublimated gas, and a recrystallization step (S530) of preferentially oversaturating the organic material, which is to be purified, of the sublimated gas, which is captured in the ionic liquid to be dissolved, to thus generate the recrystallized organic material. In the present invention, it is not necessary to perform a process of carrying the sublimated gas, which is generated during the sublimation step, to implement reverse sublimation. Accordingly, there is a merit in that the contamination of a purified sample by an inert carrier gas, which is used in a conventional sublimation purification method, is fundamentally avoided.

9. 发明申请

US20180148403A1 FENFLURAMINE COMPOSITIONS AND METHODS OF PREPARING THE SAME 审中-公开
公开(公告)号：US20180148403A1
公开(公告)日：2018-05-31
申请号：US15884742
申请日：2018-01-31
申请人： ZOGENIX INTERNATIONAL LIMITED
发明人： Derek J. LONDESBROUGH , Marc W. ANDERSEN
IPC分类号： C07C209/28 , C07C211/29 , C07C209/84 , C07C51/43 , C07C51/08 , C07C45/80 , C07C45/72
CPC分类号： C07C209/28 , C07B2200/13 , C07C45/72 , C07C45/80 , C07C51/08 , C07C51/43 , C07C209/84 , C07C211/29 , C07C57/58 , C07C49/233
摘要： Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.

10. 发明申请

US20170313805A1 TERTIARY AMINE COMPOSITION AND METHOD FOR MAKING THE COMPOSITION 审中-公开
公开(公告)号：US20170313805A1
公开(公告)日：2017-11-02
申请号：US15650596
申请日：2017-07-14
申请人： EVONIK DEGUSSA GMBH
发明人： Juan Jesus Burdeniuc , Jennifer Elizabeth Antoline Al-Rashid , Andrew Wilson Wang , Diana Sue Dunn , You-Moon Jeon , Jane Garrett Kniss , Stephan Hermann Wendel
IPC分类号： C08G18/18 , C08G18/12 , C08G18/08 , C08G18/20 , C08J9/14 , C08G18/76 , C07C209/84 , C08G18/63 , C08G18/40 , C08G18/65 , C08G101/00
CPC分类号： C08G18/1833 , C07C209/84 , C08G18/12 , C08G18/14 , C08G18/18 , C08G18/1825 , C08G18/20 , C08G18/2054 , C08G18/4072 , C08G18/4833 , C08G18/632 , C08G18/657 , C08G18/6688 , C08G18/7621 , C08G2101/0008 , C08G2101/005 , C08G2101/0083 , C08J9/14 , C08J2203/06 , C08J2205/06 , C08J2375/04 , C08J2375/08 , C08G18/3275
摘要： A composition and method for producing a tertiary amine is disclosed. The tertiary amine is contacted with an inert gas. The inert gas is nitrogen or more preferably argon. The amine composition is useful in producing polyurethane foam with lower levels of chemical emissions particularly lower emissions of toxic chemicals.

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