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Method of preparing 4-hydroxy pyrrolidone-2-acetamine

A technology for hydroxypyrrolidone and pyrrolidone, which is applied in the field of preparing 4-hydroxypyrrolidone-2-acetamide, can solve the problems that the purity cannot be fully used for medicine, cannot meet the requirements of industrial scale production, and the product composition is complicated, and the raw materials are cheap and the cost is achieved. Low cost, easy availability of raw materials

Inactive Publication Date: 2004-07-21
SUZHOU HOPE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this method, the composition of the final product is very complex, and the product needs to be adsorbed and desorbed by the resin to obtain it, and its purity cannot fully meet the requirements for medical use.
In addition, the reaction time is very long, need more than 20 hours, and its final yield is very low, such technology can not meet the needs of industrial scale production

Method used

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  • Method of preparing 4-hydroxy pyrrolidone-2-acetamine
  • Method of preparing 4-hydroxy pyrrolidone-2-acetamine
  • Method of preparing 4-hydroxy pyrrolidone-2-acetamine

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Embodiment

[0029] 1, Preparation of ethyl 4-azidoacetoacetate

[0030] 1000 ml of N,N-dimethylformamide and 167 g (1.0 mol, purity 98.5%) of ethyl 4-chloroacetoacetate were added to the reactor. Sodium azide 110g (2.0mol). The mixture was heated to 100-110°C while stirring, and reacted for 2 hours. After the reaction, the reaction mixture was cooled, and the solvent N,N-dimethylformamide was distilled and recovered under reduced pressure. Add 1000ml of water to the distillation residue, and extract with 1200ml of ethyl acetate (divided into three times, successively 600ml, 400ml, 200ml), combine several times of ethyl acetate, dry with anhydrous magnesium sulfate, and recover ethyl acetate by distillation under reduced pressure. The remainder is ethyl 4-azidoacetoacetate.

[0031] 2, Preparation of 4-hydroxyl-2-pyrrolidone

[0032] Dissolve the ethyl 4-azidoacetoacetate synthesized above in 1000ml of methanol, heat while stirring, control the temperature of the reaction mixture at 40...

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Abstract

A process for preparing 4-hydroxypyrrolidone-2-acetylamine used as brain function improver includes reacting between 4-haloacetoacetic acid derivative and the azide of alkali metal or alkali-earth metal to obtain 4-azoacetoacetic acid derivative, hydrogenating, cyclizing, and ammoniating. Its advantages are high quality and output rate of product, and low cost.

Description

technical field [0001] The invention relates to a method for preparing 4-hydroxypyrrolidone-2-acetamide. Background technique [0002] 4-Hydroxypyrrolidone-2-acetamide, commonly known as oxiracetam, is used in medicine as a brain function improver. [0003] U.S. Patents US4824861 and US4868313 describe the preparation method of oxiracetam, which are based on 3-hydroxy-4-halogenated butyric acid derivatives, with chemical reactions such as hydroxyl protection, cyclization, deprotection, and ammoniation process to prepare the desired product. [0004] The above-mentioned preparation method is not suitable for industrial scale production, because it has many disadvantages, such as the use of expensive dihydropyran as a hydroxyl protecting group, and finally the dihydropyran after removal of the protecting group is very difficult to recover. And the yield in each step of the reaction process is very low. In addition, during this reaction process, the intermediate obtained in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/12
Inventor 许国荣刘纪才
Owner SUZHOU HOPE TECH
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