Synthesis method of amisulpride impurity H

A technology for amisulpride and impurities, which is applied in the field of synthesis of amisulpride impurity H, can solve the problems of unmentioned product purity, long steps, etc., and achieves strong practical application value, few by-products, and mild reaction conditions. Effect

Pending Publication Date: 2022-05-17
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis of N-ethyl-2-methylaminomethylpyrrolidine in the patent requires 3-step reactions, the steps are long, and the purity of the product is not mentioned in the patent

Method used

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  • Synthesis method of amisulpride impurity H
  • Synthesis method of amisulpride impurity H
  • Synthesis method of amisulpride impurity H

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example 1

[0032] Synthesis of N-ethyl-2-methylaminomethylpyrrolidine

[0033] Control the temperature at 0°C and add 12.8g (0.10mol) N-ethyl-2-aminomethylpyrrolidine into 100ml of dichloromethane, then add 20.2g (0.20mol) triethylamine, add 28.3g ( 0.13mol) di-tert-butyl dicarbonate, keep 0 DEG C and react for 12 hours, wash with 100ml 10% aqueous citric acid solution, wash the organic layer with 100ml drinking water, dry the organic layer with 5g magnesium sulfate for 30 minutes, remove magnesium sulfate by filtration, The solution was cooled to 0-10°C, slowly added dropwise to the lithium aluminum hydride solution composed of 7.8g (0.2mol) lithium aluminum hydride and 100ml tetrahydrofuran, which had been cooled to 0°C in advance, heated and refluxed for 3 hours, and cooled to 0-10°C ℃, slowly added 15ml of 15% sodium hydroxide solution, stirred for 30 minutes, filtered to remove insoluble matter, and evaporated the solvent to obtain 11.4g of N-ethyl-2-methylaminomethylpyrrolidine, wi...

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Abstract

The invention belongs to the field of pharmaceutical chemicals, and relates to a synthesis method of an amisulpride impurity H. According to the invention, N-ethyl-2-methylaminomethylpyrrolidine is prepared by using a one-step method, and an impurity H is prepared by constructing an amido bond by using chloroformate and an acid-binding agent system. The method is mild in reaction condition and high in product purity, and the prepared impurity H can be used for impurity research of amisulpride.

Description

Technical field: [0001] The invention relates to a method for synthesizing the impurity H of amisulpride, which belongs to the field of medicine and chemical industry. Background technique: [0002] Amisulpride (Amisulpride, trade name Solian), alias Amisulpride, is a dopamine D3 / D2 receptor antagonist developed by Sanofi-Synthelabo (Sanofi-Synthelabo), and its chemical name is 4 -Amino-N-[(1-ethyl-2-pyrrolidinyl)methyl]-5-ethylsulfonyl-2-methoxybenzamide, the structural formula is shown in Formula I below. [0003] [0004] At present, the most commonly used synthetic method of amisulpride is to obtain it through the condensation reaction of amic acid and N-ethyl-2-aminomethylpyrrolidine, and the reaction equation is as follows: [0005] [0006] And the most conventional synthetic route of N-ethyl-2-aminomethylpyrrolidine is as follows: [0007] [0008] In the synthetic process of N-ethyl-2-aminomethylpyrrolidine, N-methylation impurity (as shown in formula II)...

Claims

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Application Information

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IPC IPC(8): C07D207/09
CPCC07D207/09
Inventor 龚玉龙李强明朱元勋颜峰峰
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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