Eureka AIR delivers breakthrough ideas for toughest innovation challenges, trusted by R&D personnel around the world.

Preparation method of carbocisteine

A technology of carbocisteine ​​and condensation reaction, which is applied in the field of preparation of carbocisteine, can solve the problems of ammonium salt or residue on ignition exceeding the standard, difficult to remove, amino acid easily exceeding the standard, etc., and achieve the reduction of impurity amino acid content, low cost, Simple operation effect

Active Publication Date: 2017-04-19
WUHAN GRAND HOYO
View PDF4 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But because L-cysteine ​​hydrochloride easily oxidizes to generate L-cystine in the raw material, and the isoelectric point of L-cystine is very close to product carbocisteine, so it is difficult to remove by refining, resulting in Other amino acids (mainly L-cystine) in the product are likely to exceed the standard; at the same time, the large amount of ammonia or sodium hydroxide used in the process will also cause the ammonium salt or residue on ignition to exceed the standard

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
  • Preparation method of carbocisteine
  • Preparation method of carbocisteine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Condensation reaction: L-cysteine ​​hydrochloride and chloroacetic acid are mixed in a molar ratio of 1: 1.1 and dissolved in water accounting for 1.5 times of the total weight of the mixture, then continuously and slowly dripping ammonia water for condensation reaction, while Slowly add sodium carbonate powder, when the pH of the reaction system rises to 3, add 0.3% Na 2 SO 3 , when the pH of the reaction system continues to rise to 5, stop adding sodium carbonate powder, when the pH of the reaction system continues to rise to 7.3, stop dripping ammonia water to end the reaction, the temperature of the entire reaction is 55 ° C, and the reaction time is 30min. The total weight of the added sodium carbonate powder accounts for 20% of the L-cysteine ​​hydrochloride weight.

[0024] (2) Neutralization and crystallization: add water accounting for 10 times the weight of L-cysteine ​​hydrochloride to the system after the condensation reaction, heat to 55°C and adjust t...

Embodiment 2

[0030] (1) Condensation reaction: L-cysteine ​​hydrochloride and chloroacetic acid are mixed at a molar ratio of 1: 1.05 and dissolved in water accounting for 2 times the total weight of the mixture, and then continuously and slowly dripping ammonia water for condensation reaction, while Slowly add sodium bicarbonate powder, and when the pH of the reaction system rises to 2.5, add 0.5% of the Na bicarbonate that accounts for the weight of L-cysteine ​​hydrochloride in one go. 2 SO 3 , when the pH of the reaction system continues to rise to 4.5, stop adding sodium bicarbonate powder, when the pH of the reaction system continues to rise to 7, stop dripping ammonia water to end the reaction, the temperature of the entire reaction is 45 ° C, and the reaction time is 40min. The total weight of the added sodium carbonate powder accounts for 10% of the L-cysteine ​​hydrochloride weight.

[0031] (2) Neutralization and crystallization: add water accounting for 7 times the weight of L...

Embodiment 3

[0034] (1) Condensation reaction: L-cysteine ​​hydrochloride and chloroacetic acid are mixed at a molar ratio of 1: 1.08 and dissolved in water accounting for 1 time of the total weight of the mixture, and then continuously and slowly dripping ammonia water for condensation reaction, while Slowly add potassium carbonate powder, and when the pH of the reaction system rises to 3.5, add 0.1% Na 2 S 2 o 5 , when the pH of the reaction system continues to rise to 5.5, stop adding potassium carbonate powder, when the pH of the reaction system continues to rise to 7.5, stop dripping ammonia water to end the reaction, the temperature of the entire reaction is 60 ° C, and the reaction time is 20min. The total weight of the added sodium carbonate powder accounts for 30% of the L-cysteine ​​hydrochloride weight.

[0035] (2) Neutralization and crystallization: add water accounting for 15 times the weight of L-cysteine ​​hydrochloride to the system after the condensation reaction, heat ...

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 preparation method of carbocisteine. The preparation method comprises the three steps of condensation reaction, neutralization and crystallization, and recrystallization. Through adding carbonate and an antioxidant to a reaction system and strictly controlling reaction conditions, the content of impurity amino acid in a finished product is reduced substantially, and the purity and the product quality of carbocisteine are improved. The preparation method has the advantages of simplicity in operation, short production cycle, low cost, and the like.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a preparation method of carbocisteine. Background technique [0002] Carboxymethylcysteine ​​(S-CMC), chemical name S-carboxymethyl-L-cysteine, molecular formula: C 5 h 9 NO 4 S, molecular weight: 179.19, structural formula as follows: [0003] [0004] Carbocisteine ​​is a sputum-eliminating drug used for the treatment of difficult expectoration caused by acute and chronic bronchitis, emphysema, tuberculosis and other diseases. [0005] There are many synthetic routes of carbocisteine. At present, industrial production mainly adopts L-cysteine ​​hydrochloride and chloroacetic acid to generate carbocisteine ​​by condensation reaction under ammonia water or liquid ammonia or sodium hydroxide solution. The crude product obtained is crystallized and recrystallized to obtain the pure product of carbocisteine, and the reaction formula is as follows: [0006] [0007] Thi...

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): C07C319/14C07C319/28C07C323/58
CPCC07B2200/07C07C319/14C07C319/28C07C323/58
Inventor 黄蕾李建华刘爱福李敬吴正俊
Owner WUHAN GRAND HOYO
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
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