Method for preparing 4-hydroxylethylpyrrolidone-2-acetamide
A technology for hydroxypyrrolidone and acetamide, which is applied in the field of preparing 4-hydroxypyrrolidone-2-acetamide, which can solve the problems that the melting point of 166-169°C cannot be fully achieved, the industrial scale production cannot be satisfied, and the product components are complex, and the cost is low. , cheap raw materials, easy to obtain the effect of raw materials
Active Publication Date: 2011-08-24
南通宏信化工有限公司
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Problems solved by technology
However, in this method, there are many side reactions, and the composition of the final product is very complex. After refining, its purity and melting point of 162-164°C cannot fully meet the requirements of medical use with a melting point of 166-169°C.
And its final yield is very low, can not meet the needs of industrial scale production
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[0024] The present invention will be described in more detail with examples below, but it cannot be considered that the present invention is limited to this example.
[0025] 1, the preparation of ethyl 4-chloro 3-hydroxybutyrate (three kinds of preparation methods are listed)
[0026] A. Add 500 ml of ethanol and 84.8 g (0.5 mol, purity 97%) of ethyl 4-chloroacetoacetate into the reactor. The mixture was cooled to 3-8°C while stirring, and 6.75 g (0.125 mol) of potassium borohydride was added to react for 6 hours. Gas chromatographic analysis obtained ethyl 4-chloro-3 hydroxybutyrate with a concentration of 12.9%, ethyl 4-chloroacetoacetate with a concentration of 0.08%, and a yield of 88.44%;
[0027] B. Add 500 ml of ethanol and 84.8 g (0.5 mol, purity 97%) of ethyl 4-chloroacetoacetate into the reactor. The mixture was cooled to 10-15°C while stirring, and 6.75 g (0.125 mol) of potassium borohydride was added to react for 6 hours. Gas chromatographic analysis obtained e...
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Abstract
The invention discloses a method for preparing oxiracetam (4-hydroxylethylpyrrolidone-2-acetamide) used for improving brain functions. The method comprises the following the steps: taking 4-chloroacetoacetic ester, ammonia, haloacetamides and the like as raw materials, conducting the steps such as hydrogenation, cyclization and the like on the 4-chloroacetoacetic ester, and finally synthesizing and obtaining the objective product; and the preparation method has the advantages that the technical process is simplified, the cost is lower, and the price of the raw materials is cheap and the raw materials are easy to obtain, and compared with the prior art, the yield rate is higher, thus being more suitable for the industrialized scale production.
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] In Japanese Patent JP62026267, it is proposed to directly react 3-hydroxy-4-halogenated butyric acid derivatives with glycinamide to prepare the target product oxiracetam. However, in this method, there are many side reactions, and the composition of the final product is very complex. After refining, its purity and melting point of 162-164°C cannot fully meet the requirements of the melting point of 166-169°C for medical use. And its final yield is very low, can not meet the needs of industrial scale production. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a method for preparing oxiracetam with lower cost, higher yield and simple operation. [0005] The ...
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IPC IPC(8): C07D207/273
Inventor 陈小萍黄卫一夏秋霞刘纪才
Owner 南通宏信化工有限公司