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Synthesis method for organic synthesis of intermediate N-acetyl-DL-methionine

A technology of organic synthesis and synthesis method, applied in organic chemistry, sulfide preparation, etc., can solve the problems of low final yield and complicated process, achieve the effect of shortening reaction time, reducing intermediate links, and improving reaction yield

Inactive Publication Date: 2018-07-06
CHENGDU DONG DIAN AI ER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But existing synthetic method adopts acetic acid to do reactant mostly, and process is more complicated, and final yield is not very high, therefore, be necessary to propose a kind of new synthetic method, this is for further improving the quality of product and yield, reduces By-product content is economically important

Method used

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  • Synthesis method for organic synthesis of intermediate N-acetyl-DL-methionine

Examples

Experimental program
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Effect test

example 1

[0011] Add 3 mol of DL-methionine to 4 mol of 4-bromo-acetanilide and heat to dissolve, add 4 mol of bromoethylamine, reflux for 90 min, add 300 ml of 30% ethanol solution, concentrate and evaporate to dryness, and reduce the temperature of the residue to 10°C, wash with 75% toluene solution, 85% nitroethane solution, recrystallize in 90% butanol solution, and dehydrate with anhydrous magnesium sulfate dehydrating agent to obtain the finished product N- Acetyl-DL-methionine 509.97g, yield 89%.

example 2

[0013] Add 3 mol of DL-methionine to 4.5 mol of 4-bromo-acetanilide and heat to dissolve, add 4.5 mol of bromoethylamine, reflux for 110 min, add 300 ml of ethanol solution with a mass fraction of 32%, concentrate and evaporate to dryness, and heat the residue to Reduce to 12°C, wash with 77% toluene solution, 87% nitroethane solution, recrystallize in 93% butanol solution, and dehydrate with anhydrous calcium sulfate dehydrating agent to obtain the finished product N-acetyl-DL-methionine 521.43g, yield 91%.

example 3

[0015] Add 3 mol of DL-methionine to 5 mol of 4-bromo-acetanilide and heat to dissolve, add 5 mol of bromoethylamine, reflux for 120 min, add 300 ml of ethanol solution with a mass fraction of 35%, concentrate and evaporate to dryness, and reduce the temperature of the residue to 15°C, wash with 80% toluene solution, 90% nitroethane solution, recrystallize in 96% butanol solution, and dehydrate with dehydrating agent to obtain the finished product N-acetyl-DL- Methionine 538.62g, yield 94%.

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Abstract

The invention relates to a synthesis method for organic synthesis of an intermediate N-acetyl-DL-methionine. The method mainly includes the steps of: adding 3mol DL-methionine into 4-5mol 4-bromo-acetanilide for heating dissolution, adding 4-5mol bromoethylamine, conducting reflux for 90-120min, adding a 300ml ethanol solution, carrying out concentration and evaporation to dryness, lowering the temperature of the residue to 10-15DEG C, performing washing with a toluene solution, conducting washing with a nitroethane solution, conducting recrystallization in a butanol solution, and performing dehydration with a dehydrant, thus obtaining the finished product N-acetyl-DL-methionine.

Description

technical field [0001] The invention relates to a synthesis method of an organic synthesis intermediate N-acetyl-DL-methionine. Background technique [0002] N-acetyl-DL-methionine is an important fine organic chemical intermediate, widely used in medicine, pesticide, chemical industry and other fields. But existing synthetic method adopts acetic acid to do reactant mostly, and process is more complicated, and final yield is not very high, therefore, be necessary to propose a kind of new synthetic method, this is for further improving the quality of product and yield, reduces The by-product content is of great economic importance. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of organic synthesis intermediate N-acetyl-DL-methionine, comprising the steps: [0004] (i) Add 3 mol of DL-methionine to 4-5 mol of 4-bromo-acetanilide and heat to dissolve, add 4-5 mol of bromoethylamine, reflux for 90-120 min, add...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/59C07C319/20
CPCC07C319/20C07C323/59
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH