CRYSTALLIZATION SEPARATION METHOD FOR NEBIVOLOL HYDROCHLORIDE INTERMEDIATE MIXTURE - SHANGHAI SHYNDEC PHARMACEUTICAL (HAIMEN) CO LTD

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%.

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Inventors:

ZHANG DONGYA (CN)
TANG QIYUN (CN)
TANG HONGYE (CN)
YU ZHENPENG (CN)
HE KANGYONG (CN)
LI HAIFENG (CN)

Application Number:

PCT/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 (CN)
SHANGHAI SHYNDEC PHARMACEUTICAL CO LTD (CN)

International Classes:

C07D311/20; C07B57/00; C07D407/04

Domestic Patent References:

WO2011009628A1	2011-01-27
WO2008010022A2	2008-01-24

Foreign References:

CN103910704A	2014-07-09
CN105085499A	2015-11-25
EP0334429A1	1989-09-27
CN101463024A	2009-06-24

Attorney, Agent or Firm:

CHINA WISPRO INTELLECTUAL PROPERTY LLP. (CN)

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