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Title:
CRYSTALLIZATION SEPARATION METHOD FOR NEBIVOLOL HYDROCHLORIDE INTERMEDIATE MIXTURE
Document Type and Number:
WIPO Patent Application WO/2017/024980
Kind Code:
A1
Abstract:
Disclosed is a crystallization separation method for a nebivolol hydrochloride intermediate mixture, which comprises the following steps: step 1, adding an alcohol solvent or a mixed solvent of an alcohol and an alkane to a nebivolol hydrochloride intermediate mixture, dissolving same into a clear solution at normal temperature, then lowering the temperature and crystallizing same, and filtering same to obtain an SS/RR type solid; and step 2, concentrating a mother solution after crystallization and filtration in step 1 until dry, then adding the alcohol solvent or the mixed solvent of an alcohol and an alkane, raising the temperature and dissolving same into a clear solution, then lowering the temperature and crystallizing same, and filtering same to obtain an RS/SR type solid. The SS/RR type and RS/SR type diastereomers in the intermediate mixture are separated by using crystallization; the operation is simple, the preparation period is relatively short, at the same time, the solvent consumption is decreased, the production cost and the aftertreatment cost of the solvent are reduced, which are conducive to realizing industrial production, and a single-pass yield of a product obtained by the separation can reach 35%-70%.

Inventors:
ZHANG, Dongya (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
TANG, Qiyun (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
TANG, Hongye (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
YU, Zhenpeng (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
HE, Kangyong (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
LI, Haifeng (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
Application Number:
CN2016/093201
Publication Date:
February 16, 2017
Filing Date:
August 04, 2016
Export Citation:
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Assignee:
SHANGHAI SHYNDEC PHARMACEUTICAL (HAIMEN) CO., LTD (No.1, Linjiang Avenue Linjiang Town, Haime, Nantong Jiangsu 6, 516006, CN)
SHANGHAI SHYNDEC PHARMACEUTICAL CO., LTD. (The Land To Build 378, Pudong New Area, Shanghai 6, 516006, CN)
International Classes:
C07D311/20; C07B57/00; C07D407/04
Domestic Patent References:
WO2011009628A12011-01-27
WO2008010022A22008-01-24
Foreign References:
CN103910704A2014-07-09
CN105085499A2015-11-25
EP0334429A11989-09-27
CN101463024A2009-06-24
Attorney, Agent or Firm:
CHINA WISPRO INTELLECTUAL PROPERTY LLP. (Room A806, Zhongdi Building China University of Geosciences Base, No.8 Yuexing 3rd Road, High-Tech Industrial Estate, Nanshan Distric, Shenzhen Guangdong 7, 518057, CN)
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