Method for synthesizing oxiracetam by adopting NaA type molecular film reactor

A membrane reactor and reaction technology, applied in the field of biomedicine, can solve the problems of low product yield, inability to reuse a large amount of water-containing ethanol, high separation energy consumption, and achieve the effects of high product yield, excellent dehydration performance and simple operation.

Pending Publication Date: 2020-07-28
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to use 4-chloro-3-hydroxybutyrate and glycinamide hydrochloride as raw materials to prepare oxiracetam by cyclization reaction, product yield is low, separation energy consumption is high and produces a large amount of hydrous ethanol The problem of not being able to be reused, using NaA type molecular sieve membrane to prepare oxiracetam by coupling vapor permeation technology and cyclization reaction

Method used

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  • Method for synthesizing oxiracetam by adopting NaA type molecular film reactor
  • Method for synthesizing oxiracetam by adopting NaA type molecular film reactor
  • Method for synthesizing oxiracetam by adopting NaA type molecular film reactor

Examples

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Effect test

Embodiment 1

[0031] Add 480 g of absolute ethanol to the reaction flask, add 55 g of glycine hydrochloride and 85 g of sodium bicarbonate under stirring, and heat up to reflux; start to drop 90 g of 4-chloro-3-hydroxybutyrate into the reaction solution, Continue to reflux and stir; when the reflux is stable, place the NaA-type molecular sieve membrane reactor above the reaction liquid, couple with the ring-closure reaction device and turn on the vacuum, the vacuum degree is 0.05Mpa, the reaction temperature and reaction time are 80°C and 24h respectively , the ratio of membrane area to reaction solution volume is 1cm 2 / cm 3 . During the reaction process, the ethanol reflux liquid was collected every 2 hours, and its water content was detected by a Karl Fischer moisture analyzer. After the cyclization reaction was completed, the reaction product was detected by high-performance liquid chromatography, and the product yield was analyzed and calculated. The water content of ethanol is shown...

Embodiment 2

[0033] Add 500 g of absolute ethanol to the reaction flask, add 60 g of glycine hydrochloride and 90 g of sodium bicarbonate under stirring, and heat up to reflux; start to drop 95 g of 4-chloro-3-hydroxybutyrate into the reaction solution, Continue to reflux and stir; when the reflux is stable, place the NaA-type molecular sieve membrane reactor above the reaction liquid, couple with the ring-closure reaction device and turn on the vacuum, the vacuum degree is 0.05Mpa, the reaction temperature and reaction time are 85°C and 24h respectively , the ratio of membrane area to reaction solution volume is 1cm 2 / cm 3 . During the reaction process, the ethanol reflux liquid was collected every 2 hours, and its water content was detected by a Karl Fischer moisture analyzer. After the cyclization reaction, the reaction product was detected by high-performance liquid chromatography, and the product yield was analyzed and calculated. The water content of ethanol is shown in the accomp...

Embodiment 3

[0035] Add 500 g of absolute ethanol to the reaction flask, add 55 g of glycine hydrochloride and 85 g of sodium bicarbonate under stirring, and heat up to reflux; start to drop 90 g of 4-chloro-3-hydroxybutyrate into the reaction solution, Continue to reflux and stir; when the reflux is stable, place the NaA-type molecular sieve membrane reactor above the reaction liquid, couple with the ring-closure reaction device and turn on the vacuum, the vacuum degree is 0.05Mpa, the reaction temperature and reaction time are 85°C and 24h respectively , the ratio of membrane area to reaction solution volume is 1cm 2 / cm 3 . During the reaction process, the ethanol reflux liquid was collected every 2 hours, and its water content was detected by a Karl Fischer moisture analyzer. After the cyclization reaction, the reaction product was detected by high-performance liquid chromatography, and the product yield was analyzed and calculated. The water content of ethanol is shown in the accomp...

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Abstract

The invention discloses a method for synthesizing oxiracetam by adopting a NaA type molecular sieve membrane reactor. According to the method, the prepared NaA molecular sieve membrane is used to prepare oxiracetam through vapor permeation technology coupled with a cyclization reaction. The method specifically comprises the following steps of: adding absolute ethyl alcohol into a reaction flask, adding glycine hydrochloride and sodium bicarbonate in a stirring state, and heating to reflux; dropwise adding 4-chloro-3-hydroxybutyrate into the reaction liquid, continuing reflux stirring until thereflux is stable, placing the NaA type molecular sieve membrane reactor above the reaction liquid to be coupled with a cyclization reaction device and start vacuum for a reaction, and thereby obtaining a reaction product after the reaction is completed. According to the method, the energy consumption required by cyclization reaction and the requirements on reaction equipment are reduced, the yield of the product and the purity in the separation process are improved, the recycling of ethanol is realized, and the production cost is saved.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, relates to a method for synthesizing oxiracetam, in particular to a method for synthesizing oxiracetam by using a NaA type molecular sieve membrane reactor. Background technique [0002] Oxiracetam, English name Oxiracetam, chemical name 4-hydroxyl-2-oxopyrrolidine-N-acetamide; 2-(4-hydroxyl-2-oxo-1-pyrrolidinyl)acetamide, the The compound can be obtained from methanol as a white microcrystalline powder with a melting point of 165-168°C. In 1974, it was synthesized for the first time by the Italian Skeleton Bichem Company, and it was launched in Italy in 1987. Its trade name is Neuromet, which is a new generation of brain metabolism improving drug. , senile dementia, vascular dementia, etc.; oxiracetam belongs to the piracetam class of drugs, and its efficacy is better than that of piracetam, and it is well tolerated and has fewer adverse reactions. [0003] At present, there have been many...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/273B01J19/18C01B39/14
CPCC07D207/273B01J19/18C01B39/14
Inventor 吴巍盖来兵臧毅华袁立盛春光陈赞王仑罗超
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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