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Method for preparing 2-amino-4-(methylthio)butyramide

A technology of methylthiobutyramide and aminobutyronitrile is applied in sulfide preparation, chemical recovery, organic chemistry and other directions, and can solve the problems of easy polymerization of nitrile, and achieve the effects of difficult polymerization, high yield and simple preparation method.

Inactive Publication Date: 2021-06-18
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem that nitriles are easily polymerized in the hydrolysis process, the invention provides a method for preparing 2-amino-4-methylthiobutyramide

Method used

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  • Method for preparing 2-amino-4-(methylthio)butyramide

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Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1 (ceria is made catalyst, the 1st batch)

[0031]Put into cyanohydrin (60g77.9%, 0.356mol) in the stainless steel autoclave that is equipped with magnetic stirrer and jacket, under the state that is heated to 30 ℃, pass into ammonia gas, control pressure 0.3-0.4MPa, at 30 Stir at ℃ for 3 hours, the consumption of ammonia is 3.5 times of the moles of cyanohydrin, and the obtained ammoniated solution containing aminobutyronitrile is flashed to remove excess ammonia, and the ammonia content is 6.3%. After deamination, add 56.7g of ammoniated solution containing aminobutyronitrile and 35g of solid catalyst cerium oxide into the reaction device, maintain 40°C for hydrolysis reaction, and react to generate 2-amino-4-methylthiobutyramide, hydrolysis time 1h . After completion of the reaction, add 390g of water, keep the heat preservation and let it stand for 0.5h to stratify. The catalyst at the bottom of the reaction device is applied mechanically to the next bat...

Embodiment 2

[0032] Embodiment 2 (ceria is made catalyst, and catalyst is applied mechanically the 1st batch)

[0033] Put into cyanohydrin (60g77.9%, 0.356mol) in the stainless steel autoclave that is equipped with magnetic stirrer and jacket, under the state that is heated to 30 ℃, pass into ammonia gas, control pressure 0.3-0.4MPa, at 30 Stir at ℃ for 3 hours, the consumption of ammonia is 3.5 times of the moles of cyanohydrin, and the obtained ammoniated solution containing aminobutyronitrile is flashed to remove excess ammonia, and the ammonia content is 5.8%. After deamination, 56.6 g of the ammoniated solution containing aminobutyronitrile was added to the reaction device containing ceria catalyst, and the hydrolysis reaction was carried out at 40 °C to generate 2-amino-4-methylthiobutyramide, and the hydrolysis time was 1 hour. After the reaction is complete, add 390g of water, keep the heat and let it stand and separate for 0.5h. The catalyst at the bottom of the reaction device i...

Embodiment 3

[0034] Embodiment 3 (ceria is made catalyst, and catalyst is applied mechanically the 2nd batch)

[0035] Put into cyanohydrin (60g77.9%, 0.356mol) in the stainless steel autoclave that is equipped with magnetic stirrer and jacket, under the state that is heated to 30 ℃, pass into ammonia gas, control pressure 0.3-0.4MPa, at 30 Stir at ℃ for 3 hours, the consumption of ammonia is 3.5 times of the moles of cyanohydrin, and the obtained ammoniated solution containing aminobutyronitrile is flashed to remove excess ammonia, and the ammonia content is 5.9%. After deamination, 57.2 g of the ammoniated solution containing aminobutyronitrile was added to the reaction device containing ceria catalyst, and the hydrolysis reaction was carried out at 40°C to generate 2-amino-4-methylthiobutyramide, and the hydrolysis time was 1 hour. After the reaction is complete, add 390g of water, keep the temperature and let it stand for 0.5h to separate layers. The catalyst at the bottom of the react...

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Abstract

The invention provides a method for preparing 2-amino-4-(methylthio)butyramide. 2-Amino-4-(methylthio)butyronitrile is prepared by taking 2-hydroxy-4-(methylthio)butyronitrile as a raw material, 2-10% of ammonia is maintained in a hydrolysis system, and then catalytic hydrolysis is conducted at a relatively low temperature to prepare 2-amino-4-(methylthio)butyramide. According to the method, a solid catalyst is used in the hydrolysis process, the 2-amino-4-(methylthio)butyramide is prepared through hydrolysis at a relatively low temperature, the catalyst is easily separated from the hydrolysate, so that the catalyst is recycled, and the service life of the catalyst is greatly prolonged. Cerium dioxide is used as a catalyst to carry out low-temperature catalytic hydrolysis reaction, high activity is still maintained after 20 times of cyclic application, and the economic benefit is obviously improved compared with the prior art.

Description

technical field [0001] The invention relates to a method for preparing 2-amino-4-methylthiobutanamide, which belongs to the technical field of fine chemicals. Background technique [0002] 2-Amino-4-methylthiobutanamide, also known as methionine, is an important chemical intermediate, which can be used to prepare antiepileptic drug levetiracetam, new antibiotic acetylglucosamine deacetylase, immune Biochemical agents such as homocysteine. At present, the production methods of 2-amino-4-methylthiobutyramide mainly include chemical synthesis, biological fermentation, and enzyme catalysis, among which chemical synthesis is the most common. The known chemical synthesis process route is to prepare 2-amino-4-methylthiobutyramide by catalytic hydrolysis of 2-amino-4-methylthiobutyronitrile (abbreviated as "aminobutyronitrile"). Since the α-position of 2-hydroxy-4-methylthiobutyronitrile ("cyanohydrin") and aminobutyronitrile has an amino group or a hydroxyl group, both the amino ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C323/60
CPCC07C319/20C07C323/60Y02P20/584
Inventor 郑道敏刘佳王冬林金海琴姚如杰罗延谷唐大家邓建伟孔雪婷徐代行柳亚玲刘丹张兰
Owner CHONGQING UNISPLENDOUR CHEM
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