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1. CN107848978 - METHOD FOR SEPARATING DIASTEREOISOMER A OF BEDAQUILINE

Office
China
Application Number 201580081471.2
Application Date 24.07.2015
Publication Number 107848978
Publication Date 27.03.2018
Grant Number 107848978
Grant Date 02.04.2021
Publication Kind B
IPC
C07D 215/227
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
DHETEROCYCLIC COMPOUNDS
215Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
02having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
16with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
20Oxygen atoms
22attached in position 2 or 4
227only one oxygen atom which is attached in position 2
C07F 1/02
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
FACYCLIC, CARBOCYCLIC, OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
1Compounds containing elements of Groups 1 or 11 of the Periodic System
02Lithium compounds
CPC
C07D 215/227
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
DHETEROCYCLIC COMPOUNDS
215Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
02having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
16with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
20Oxygen atoms
22attached in position 2 or 4
227only one oxygen atom which is attached in position 2
C07F 1/02
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
1Compounds containing elements of Groups 1 or 11 of the Periodic System
02Lithium compounds
Applicants ZHEJIANG HISUN PHARMACEUTICAL CO LTD
浙江海正药业股份有限公司
SHANGHAI INST PHARMACEUTICAL INDUSTRY
上海医药工业研究院
Inventors ZHANG FULI
张福利
PAN LINYU
潘林玉
ZHU JINJIN
朱津津
WANG XINZENG
王新增
ZHAO LI
赵立
REN ZHONG
任重
SONG YING
宋颖
Agents 北京信诺创成知识产权代理有限公司 11728
Title
(EN) METHOD FOR SEPARATING DIASTEREOISOMER A OF BEDAQUILINE
(ZH) 一种分离贝达喹啉非对映异构体A的方法
Abstract
(EN) Disclosed is a method for separating a diastereoisomer A of Bedaquiline. The method comprises the following steps: (1) adding a reversed-phase solvent into a Bedaquiline reaction liquid comprising diastereoisomers A and B, so as to precipitate out the diastereoisomer B; and (2) removing the diastereoisomer B precipitated out in step (1), so as to obtain the diastereoisomer A. The separation methodof the present invention is easy to operate and is stable, and has higher industrialization value compared with separation and purification in a conventional column chromatography method, and can resolve the problems of difficulty in purifying and separating Bedaquiline due to the small amount of a product caused by an excessively low conversion rate because preparation condition of Bedaquiline is harsh and the conversion rate is difficult to ensure; raw material residuals can be easily removed, the yield is high, and the purity of the diastereoisomer A is high, which facilitates the split; split can be further carried out to obtain a qualified Bedaquiline product with a purity greater than or equal to 99.0%, wherein the impurities of the diastereoisomers are lower than or equal to 0.1%.
(ZH) 本发明公开了一种分离贝达喹啉非对映异构体A的方法,包括如下步骤:(1)向含有非对映异构体A和B的贝达喹啉反应液中,加入反相溶剂,析出非对映异构体B;(2)除去步骤(1)析出的非对映异构体B,得到非对映异构体A。本发明的分离方法,操作简便、方法稳定;比传统的柱层析法分离纯化更有工业化价值;可克服由于贝达喹啉的制备反应条件苛刻,转化率难以保证,进而导致转化率低时产物量少而难以对其进行纯化分离的技术问题;可轻易地去除原料残留,收率高、非对映异构体A的纯度也高,有利于拆分,经进一步拆分可制备得到合格的贝达喹啉终产物,纯度≥99.0%,其中非对映异构体杂质≤0.1%。
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