Preparation method of tianeptine sodium impurity D

A technology for tianeptine sodium and impurities, which is applied in the field of preparation of tianeptine sodium impurity D, can solve problems such as no public data report on the synthesis method of impurity D, achieve high purity and solve the problems of quality control.

Active Publication Date: 2013-03-20
SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are 5 impurities in the quality standard of tianeptine sodium in the BP2009 version, of which impurity D is not sold in the market, and there is no public information on the synthesis method of impurity D

Method used

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  • Preparation method of tianeptine sodium impurity D
  • Preparation method of tianeptine sodium impurity D

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 30.7g 3-chloro-6-methyldibenzo[c,f][1,2]thiazepine-11(6H)-one S,S-dioxide and 18.2g 7-aminoheptanoate Add salt to 153.5ml of toluene, add 8g of sodium hydroxide, heat and reflux for 5 hours, after the reaction is completed, cool to room temperature, adjust pH=5~6 with 1N dilute hydrochloric acid, filter, wash with a small amount of ethanol, and dry to obtain 36g of crude product.

[0016] ②Add 36g of the crude product to 180ml of ethanol, heat to reflux for 30 minutes, cool to room temperature, filter, and dry to obtain 30.8g of pure impurity D, with a purity greater than 99.5% and a total yield of 71%.

Embodiment 2

[0018] 61.4g3-chloro-6-methyldibenzo[c,f][1,2]thiazepine-11(6H)-one S,S-dioxide and 40g 7-aminoheptanoic acid hydrochloride Add salt to 368.4ml of toluene, add 17.6g of sodium hydroxide, heat and reflux for 6 hours, after the reaction is complete, cool to room temperature, adjust pH=5~6 with 1N dilute hydrochloric acid, filter, wash with a small amount of ethanol, and dry to obtain 73g of crude product.

[0019] ②Add 73g of the crude product to 438ml of ethanol, heat to reflux for 30 minutes, cool to room temperature, filter, and dry to obtain 62.2g of pure impurity D, with a purity greater than 99.5%, and a total yield of 71%.

Embodiment 3

[0021] 200g 3-chloro-6-methyldibenzo[c,f][1,2]thiazepine-11(6H)-one S,S-dioxide and 130g 7-aminoheptanoate hydrochloride Add 1.1L of toluene, add 57g of sodium hydroxide, heat and reflux for 5.5 hours, after the reaction is completed, cool to room temperature, adjust pH=5~6 with 1N dilute hydrochloric acid, filter, wash with a small amount of ethanol, and dry to obtain 238g of crude product.

[0022] ②Add 238g of the crude product to 1.3L of ethanol, heat to reflux for 30 minutes, cool to room temperature, filter, and dry to obtain 203g of pure impurity D, with a purity greater than 99.5%, and a total yield of 72%.

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Abstract

The invention relates to a preparation method of tianeptine sodium impurity D. The 3-chlorine-6-methyl dibenzo [c, f][1, 2] thiazepine-11 (6H)- ketone S, S-dioxide and 7-amino heptylic acid hydrochloride are used as starting materials, a crude product is prepared by dehydration under alkaline condition, and the crude product is refined to prepare the 7-[(3-chlorine-6,11- dihydro-6- methyl dibenzo [c, f][1,2] thiazepine-11-yl)- imino group]- heptylic acid S, S-dioxide, namely the tianeptine sodium impurity D. The preparation method provided by the invention is short in synthetic route, simple to operate and high in product purity, and can provide qualified reference sample for the quality control of tianeptine sodium.

Description

technical field [0001] The invention relates to medicines, and relates to a preparation method of impurity D of tianeptine sodium. Background technique [0002] Tianeptine sodium is a drug for the treatment of mental disorders produced by the French Servier International Company. The chemical name is 7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]-thiazepin-11-yl)-amino]heptanoic acid S, S-dioxide sodium salt, the trade name is Datilang. This product was launched in the domestic market in 2001. It is used for the treatment of mild, moderate or severe depression, neurogenic and reactive depression, anxiety and depression with physical discomfort, especially gastrointestinal discomfort, and alcohol dependence patients during the withdrawal process. anxiety and depression. [0003] The related research on the impurities of tianeptine sodium is very important, it can be used for the qualitative and quantitative analysis of impurities in the production of tianeptine sodium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D281/02
Inventor 宋文同王树力谢彩霞
Owner SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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