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Method for preparing (S)-2-aminobutanamide hydrochloride

A technology of aminobutyramide and hydrochloride, which is applied in the preparation of carboxylic acid amide, optical isomers of carboxylic acid amide, and preparation of organic compounds, etc. It can solve air pollution, high risk of production operation, and S-2 aminobutyramide High acid prices and other issues, to achieve the effects of no air pollution, less risk in production operations, and low production costs

Inactive Publication Date: 2013-01-30
FUXIN LONGRUI CHEM CO LTD
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Problems solved by technology

[0003] The synthetic method mainly contains the following two kinds: 1) n-propionaldehyde reacts with hydrocyanic acid and ammonia water to generate a Streck reaction to generate 2-aminobutyronitrile hydrolysis to obtain 2-aminobutanamide salt, but this method uses highly toxic hydrogen Cyanic acid, the risk of production operation is relatively high, and the air pollution is serious
2) With the chiral compound S-2 aminobutyric acid as the starting material, S-2 aminobutyramide hydrochloride is obtained through esterification and aminolysis. This method can avoid the resolution process and the product has high purity, but S-2 GABA is more expensive

Method used

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  • Method for preparing (S)-2-aminobutanamide hydrochloride
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  • Method for preparing (S)-2-aminobutanamide hydrochloride

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Embodiment Construction

[0018] The present invention will be described in detail below in conjunction with specific embodiments.

[0019] 1. Ammonification:

[0020] Reaction equation:

[0021] 5000 kilograms of ammoniacal liquor are added in the ammoniation still from the ammoniacal liquor tank, add 2-bromobutyrate methyl 800kg when opening the ammoniation still jacket freezing brine and cooling to-5 DEG C. -5°C--5°C temperature controlled reaction for 2 hours, the system was naturally heated to 45°C, sampled for analysis, high-pressure liquid phase analysis 2-bromobutyrate methyl ester reaction was completed and the reaction was terminated.

[0022] Add the ammoniated solution into the still, open the jacket steam to raise the temperature to 50°C, discharge the ammonia gas into the ammonia water storage tank (open the jacket cooling water in the ammonia water storage tank to cool down), after the ammonia discharge is completed, raise the temperature to 80°C, and distill and recover the reaction ...

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Abstract

The invention discloses a method for preparing (S)-2-aminobutanamide hydrochloride. The method comprises the following steps of: A1, ammoniating; A2, splitting; and A3, salifying: starting a salifying reaction kettle jacket for refrigerating a salt solution, adding hydrogen chloride isopropanol, cooling to 5 DEG C below zero, adding (S)-2-aminobutanamide tartrate obtained by splitting in batches, heating and refluxing for 2 hours, cooling, and centrifuging to obtain (S)-2-aminobutanamide hydrochloride, wherein the molar ratio of 2-aminobutanamide hydrochloride to hydrogen chloride isopropanol is 1:1.5. The method has the advantages of no use of virulent hydrocyanic acid, low production operation risk, prevention of air pollution, high product purity and low production cost.

Description

technical field [0001] The invention relates to a preparation method of (S)-2-aminobutanamide hydrochloride. Background technique [0002] (S)-2-Aminobutanamide hydrochloride is an important intermediate of the new auxiliary antiepileptic drug levetiracetam, and there is a large demand in the international market. The chemical name of levetiracetam is (S)-α-ethyl-2-oxo-1-pyrrolidineacetamide, molecular formula: C8H14N2O2, molecular weight: 170.21. [0003] The synthetic method mainly contains the following two kinds: 1) n-propionaldehyde reacts with hydrocyanic acid and ammonia water to generate a Streck reaction to generate 2-aminobutyronitrile hydrolysis to obtain 2-aminobutanamide salt, but this method uses highly toxic hydrogen Cyanic acid, the risk of production operation is relatively high, and the air pollution is serious. 2) With the chiral compound S-2 aminobutyric acid as the starting material, S-2 aminobutyramide hydrochloride is obtained through esterification ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/06C07C231/20C07C231/14
Inventor 杨占杰马岩程恩喜
Owner FUXIN LONGRUI CHEM CO LTD
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