Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Synthesis method of DL-cysteine

A synthesis method and cysteine ​​technology, applied in the field of DL-cysteine ​​synthesis, can solve the problems of high toxicity and high price, and achieve the effects of reaction safety, short reaction steps and simple reaction operation.

Active Publication Date: 2021-02-12
山东嘉成医药科技有限公司
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials ethyleneimine, bromine, and cyanide involved in the above reactions are expensive or highly toxic;

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis method of DL-cysteine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The synthetic method of embodiment 1 DL-cysteine, refer to figure 1 As shown, the details are as follows:

[0028] (1) Add 50g of acrylonitrile to a three-necked reaction flask, add catalyst magnesium carbonate, the amount of catalyst used is 10% of the weight of acrylonitrile, and slowly introduce 70g of chlorine gas below 0°C to maintain the reaction temperature between 12°C and chlorine gas After passing through, it was incubated at 12°C for 3 hours, then fed into nitrogen to drive off excess chlorine gas, and the reaction ended to obtain 114.7g of 2,3-dichloropropionitrile ( figure 1 The middle mark is 1), the yield is 98.1%, and the purity is 98.4%;

[0029] (2) Add a mixed medium of 85% acetic acid, concentrated sulfuric acid and water with a volume ratio of 1:1:1.2 to the reaction flask, then add 100 g of 2,3-dichloropropionitrile prepared in step (1), and then Reflux at 115°C for 1 hour to obtain 102.6 g of 2,3-dichloropropionic acid ( figure 1 The winning nu...

Embodiment 2

[0033] The synthetic method of embodiment 2 DL-cysteine, refer to figure 1 As shown, the details are as follows:

[0034] (1) Add 50g of acrylonitrile to a three-necked reaction flask, add catalyst magnesium carbonate, the amount of catalyst used is 12% of the weight of acrylonitrile, slowly introduce 70g of chlorine gas below 3°C, keep the reaction temperature between 17°C, chlorine gas After passing through, it was incubated at 17° C. for 4 hours, then fed into nitrogen to drive out excess chlorine, and the reaction ended to obtain 107 g of 2,3-dichloropropionitrile ( figure 1 The middle mark is 1), the yield is 92%, and the purity is 99%;

[0035] (2) Add a mixed medium of 85% acetic acid, concentrated sulfuric acid and water with a volume ratio of 1:1:1.2 to the reaction flask, then add 100 g of 2,3-dichloropropionitrile prepared in step (1), and then Reflux at 120°C for 1.2 hours to obtain 100.8 g of 2,3-dichloropropionic acid ( figure 1 The winning number is 2), the y...

Embodiment 3

[0039] The synthetic method of embodiment 3 DL-cysteine, refer to figure 1 As shown, the details are as follows:

[0040] (1) Add 50g of acrylonitrile to a three-necked reaction flask, add catalyst magnesium carbonate, the amount of catalyst used is 11% of the weight of acrylonitrile, slowly introduce 70g of chlorine gas below 0°C, and keep the reaction temperature between 14°C and chlorine gas After passing through, keep warm at 14 DEG C for 3 hours, then feed nitrogen to drive off excess chlorine, and the reaction ends to obtain 115g of 2,3-dichloropropionitrile ( figure 1 The middle mark is 1), the yield is 98.4%, and the purity is 98.9%;

[0041] (2) Add a mixed medium of 85% acetic acid, concentrated sulfuric acid and water with a volume ratio of 1:1:1.2 to the reaction flask, then add 100 g of 2,3-dichloropropionitrile prepared in step (1), and then Reflux at 118°C for 1.2 hours to obtain 104 g of 2,3-dichloropropionic acid ( figure 1 The middle mark is 2), the yield ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a synthetic method of DLcysteine. The method comprises the following steps: by using acrylonitrile as a raw material, chlorinating to generate 2, 3dichloropropionitrile, hydrolyzing to generate corresponding acid, reacting the acid with thiourea to cyclize to generate 2-aminothiazoline-4-carboxylic acid, adding alkali sulfide to generate 2-mercaptothiazoline-4-carboxylic acid, and hydrolyzing to generate cysteine. The synthesis method provided by the invention has the advantages of short synthesis steps, mild preparation conditions, sufficient and cheap raw material sources and higher product yield.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a synthesis method of DL-cysteine ​​with short reaction steps, mild reaction conditions and high yield. Background technique [0002] Cystine is usually produced from animal hair by hydrolysis. On the one hand, animal hair is used as raw material, and the yield is extremely low, and waste disposal is difficult, causing environmental pollution; on the other hand, L-cystine is produced by hydrolysis. Cystine is widely used in medicine, cosmetics, food nutrition enhancers and other fields. In recent years, the application demand has increased significantly, not limited to L-cystine or L-cysteine, D-cystine (or D-cysteine Cystine) also has corresponding applications, such as the synthetic drug cefminol, and its derivative D-s-(p-methoxybenzyl)cysteine ​​is an important component of the HIV inhibitor KNI764. N-acetylcysteine ​​can be used to promote skin wound cell...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/02C07C323/58C07D277/18C07D277/16C07C51/08C07C53/19C07C253/30C07C255/10
CPCC07C319/02C07D277/18C07D277/16C07C51/08C07C253/30C07C255/10C07C53/19C07C323/58Y02P20/52
Inventor 王平生
Owner 山东嘉成医药科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com