Title:
MINOCYCLINE(II) P-CHLOROBENZENE SULFONATE CRYSTAL FORM, PREPARATION METHOD THEREFOR AND USE THEREOF
Document Type and Number:
WIPO Patent Application WO/2020/135508
Kind Code:
A1
Abstract:
Disclosed are a minocycline(II) p-chlorobenzene sulfonate crystal form, a preparation method therefor and the use thereof. In the current preparation process of minocycline hydrochloride, the last step, i.e. the post-treatment and purification operations of a hydrogenation reaction, is the bottleneck part of the process. The preparation method for the minocycline(II) p-chlorobenzene sulfonate crystal form of the present invention comprises the following steps: dissolving a hydrogenation azo substance in an alcohol solvent, adding an acid and a palladium carbon catalyst, displacing same with nitrogen gas, and then subjecting same to a hydrogenation reaction, then adding formaldehyde at a mass percent of 35-40%, and continuously subjecting same to a hydrogenation reaction; and after the reaction is finished, displacing same with nitrogen gas, filtering the catalyst, adding p-chlorobenzenesulfonic acid for crystallization, slowly decreasing the temperature to an endpoint temperature, and filtering and drying same. The preparation method of the present invention is simple and convenient, and stable, is suitable for industrialization, and is also beneficial for subsequent filtering and drying operations. For the prepared minocycline(II) p-chlorobenzene sulfonate crystal form, the product quality thereof is sufficient for raw material drugs for preparing minocycline hydrochloride which meets required standards.
Inventors:
LIU LUO (CN)
WU GUOFENG (CN)
SHEN XIANGLI (CN)
YU TENGFEI (CN)
JIN JIANQING (CN)
LI LIANG (CN)
XIE BIN (CN)
LI WEI (CN)
CHEN LONG (CN)
WU GUOFENG (CN)
SHEN XIANGLI (CN)
YU TENGFEI (CN)
JIN JIANQING (CN)
LI LIANG (CN)
XIE BIN (CN)
LI WEI (CN)
CHEN LONG (CN)
Application Number:
PCT/CN2019/128333
Publication Date:
July 02, 2020
Filing Date:
December 25, 2019
Export Citation:
Assignee:
ZHEJIANG CHANGHAI PHARMACEUTICAL CO LTD (CN)
ZHEJIANG MEDICINE CO LTD XINCHANG PHARMACEUTICAL FACORTY (CN)
ZHEJIANG MEDICINE CO LTD XINCHANG PHARMACEUTICAL FACORTY (CN)
International Classes:
C07C237/26; C07C231/12
Foreign References:
| CN101228111A | 2008-07-23 | |||
| US3483251A | 1969-12-09 | |||
| CN103387512A | 2013-11-13 | |||
| CN107108472A | 2017-08-29 |
Attorney, Agent or Firm:
ZHEJIANG SHINE PATENT OFFICE (GENERAL PARTNER) (CN)
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