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Preparation method of environment-friendly and high-purity sulpiride

An environmental protection and nitrogen protection technology is applied in the field of preparation of environmentally friendly high-purity sulpiride, which can solve the problems of low purity of sulpiride, sewage, time-consuming and labor-intensive, etc., and achieve the effects of high degree of crystal precipitation, reduced waste, and high yield.

Inactive Publication Date: 2018-07-31
大桐制药(中国)有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis method of sulpiride has been reported in many documents, and ethylene glycol is mostly used as a solvent for preparation, and then it is obtained by washing with water after filtration, but in the preparation process, it is time-consuming and laborious, and a large amount of sewage containing organic matter is produced, and the obtained sulpiride The purity of the product is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of environment-friendly high-purity sulpiride, comprising the steps of:

[0023] S1, crude product preparation

[0024] Put 10g of methyl 2-methoxy-5-sulfamoylbenzoate and 5g of N-ethyl-2aminomethyltetrahydropyrrolidine into the reaction vessel, add 104g of glycerol, and react at a temperature of 91°C under nitrogen protection 2h, add 210g of water and stir for 24min, cool down to room temperature, stop feeding nitrogen, continue to cool down to 0°C, let stand for 11min, filter and dry to obtain the crude product;

[0025] S2, bamboo charcoal activation

[0026] 10g of bamboo powder was fermented with 1.2g of EM bacterial liquid for 11 days, dried, pulverized, immersed in a 1.2mol / L sodium hydroxide solution and allowed to stand for 21 hours, filtered, dried, and placed in a vacuum box at a temperature of 802°C for 22 minutes. Cool down to room temperature at a rate of 0.2°C / min, wash until neutral, dry, and pulverize to obtain activated bamboo ch...

Embodiment 2

[0030] A preparation method of environment-friendly high-purity sulpiride, comprising the steps of:

[0031] S1, crude product preparation

[0032] Send 20g of 2-methoxy-5-sulfamoylbenzoic acid methyl ester and 10g of N-ethyl-2 aminomethyltetrahydropyrrolidine into the reaction vessel, add 135g of glycerol, and react at a temperature of 94°C under nitrogen protection 4h, add 380g of water and stir for 38min, cool down to room temperature, stop feeding nitrogen, continue to cool down to 2°C, let stand for 18min, filter and dry to obtain the crude product;

[0033] S2, bamboo charcoal activation

[0034] 10g of bamboo powder was fermented with 2g of EM bacterial liquid for 19 days, dried, pulverized, immersed in a 1.4mol / L sodium hydroxide solution and allowed to stand for 28h, filtered, dried, put into a vacuum box and kept at a temperature of 825°C for 36min. Cool down to room temperature at a rate of 0.7°C / min, wash until neutral, dry, and pulverize to obtain activated bamb...

Embodiment 3

[0038] A preparation method of environment-friendly high-purity sulpiride, comprising the steps of:

[0039] S1, crude product preparation

[0040] Put 14g of 2-methoxy-5-sulfamoylbenzoic acid methyl ester and 8g of N-ethyl-2 aminomethyltetrahydropyrrolidine into the reaction vessel, add 120g of glycerin, and react at a temperature of 93°C under nitrogen protection 3h, add 320g of water and stir for 32min, cool down to room temperature, stop feeding nitrogen, continue to cool down to 1°C, let stand for 16min, filter and dry to obtain the crude product;

[0041] S2, bamboo charcoal activation

[0042] 10g of bamboo powder was fermented with 1.4g of EM bacterial liquid for 16 days, dried, pulverized, immersed in a 1.3mol / L sodium hydroxide solution and allowed to stand for 26h, filtered, dried, and put into a vacuum box at a temperature of 825°C for 32min. Cool down to room temperature at a rate of 0.4°C / min, wash until neutral, dry, and pulverize to obtain activated bamboo ch...

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Abstract

The invention discloses a preparation method of environment-friendly and high-purity sulpiride. The preparation method comprises the following steps of preparation of a crude product; activation of bamboo charcoal, wherein, in the activation process of the bamboo charcoal, fermenting bamboo powder by adopting EM (Effective Microorganism) bacterial liquid, drying, crushing, immerging in a sodium hydroxide solution, standing, filtering, drying, sending into a vacuum box, activating at a high temperature, washing until being neutral, drying and crushing, so that activated bamboo charcoal is obtained; purification of the coarse product: in the purification process of the crude product, adding absolute ethyl alcohol into the crude product, refluxing at a temperature of 80 to 100 DEG C, coolingthe temperature to 0 to 2 DEG C, filtering, adding an ethyl alcohol solution with a concentration of 80wt% to 95wt%, refluxing at the temperature of 80 to 100 DEG C, adding the activated bamboo charcoal, continuously refluxing, ultrasonically treating, filtering, crystallizing, and carrying out vacuum drying, so that the environment-friendly and high-purity sulpiride is obtained. A product obtained by the preparation method is high in purity and yield; the preparation technique is simple; the use level of an organic matter in a preparation process is low; in addition, the ethyl alcohol in a rejected material is easily recovered and can be further repeatedly utilized; the waste to a resource and the pollution to an environment can be reduced, and the preparation method is safe and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of preparation of sulpiride, in particular to a preparation method of environment-friendly high-purity sulpiride. Background technique [0002] Sulpiride, also known as thiobenzamide, Shuning, antiemetic or Xiaovoning, is a benzamide antipsychotic drug, which can be used for depressive state of schizophrenia, symptomatic psychosis, functional depression and hypochondriac state, alcoholism Mental illness, mental retardation accompanied by personality disorder, senile mental illness, especially patients with symptoms such as apathy, withdrawal, stupor, depression, hallucinations, doubts and delusions, and it is a central antiemetic drug with a strong antiemetic effect effect. At present, the synthesis method of sulpiride has been reported in many documents, and ethylene glycol is mostly used as a solvent for preparation, and then it is obtained by washing with water after filtration, but in the preparation pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/09
CPCC07D207/09
Inventor 张艳华张媛张荣玉
Owner 大桐制药(中国)有限责任公司
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