7-ADCA recovery method

A technology of 7-ADCA and recovery method, applied in the field of 7-ADCA recovery, can solve the problems of low yield and low recovery rate of cefadroxil naphthol complex, and achieves convenient operation, obvious safety and environmental protection benefits, and improved product quality Effect

Active Publication Date: 2021-11-26
ZHEJIANG ANGLIKANG PHARMA
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the further purification of the cefadroxil naphthol compound still needs to use organic solvents, and the pollution still exists; on the other hand, the recovery rate of the cefadroxil naphthol compound is not high and the yield is low

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
  • 7-ADCA recovery method
  • 7-ADCA recovery method
  • 7-ADCA recovery method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Influence of additive dosage on reaction effect in pretreatment

[0033] In the pretreatment process, there are two main additives: EDTA and sodium bisulfite.

[0034] In the following, in combination with the specific recovery process, the experiment is first carried out on the influence of the dosage of EDTA.

[0035] (1) Add 1000ml of cefadroxil crystallized mother liquor prepared by the enzymatic cefadroxil process route into the reactor with stirring, the concentration of cefadroxil is about 15mg / ml, heat up to 15°C, control the dosage of EDTA, sulfurous acid Sodium hydrogen 0.20g, adjust the pH of the mother liquor to 7.0 with ammonia water, stir for later use.

[0036] (2) A self-designed bioreactor, put an appropriate amount of immobilized biological enzyme 15g into the bioreactor, put it into the feed liquid configured in (1), use ammonia water for enzyme reaction to maintain pH 7.0, temperature 15°C, every 1 hour Sampling inspection, using high pe...

Embodiment 2

[0053] Example 2: Influence of parameters on reaction effect in pretreatment

[0054] Enzyme-catalyzed reactions need to be at a suitable temperature to exhibit the best catalytic activity. If the temperature is too low, the enzyme activity is not high. The main temperature affects the contact probability between the substrate molecule and the catalytic center of the enzyme activity. The higher the temperature, the more intense the molecular motion and the higher the probability of contacting the catalytic center. On the other hand, if the temperature is too high, It will also change the spatial conformation of the enzyme molecule, denaturing and inactivating. At the same time, too high temperature leads to accelerated degradation of cephalosporins and darker color, so it is necessary to pretreat the temperature of the feed liquid in an appropriate range. The pretreatment of this step is to provide suitable conditions for the next enzyme reaction, so the temperature is tested...

Embodiment 3

[0081] Example 3: Effect of Immobilized Enzyme Dosage on Reaction Effect

[0082] As a catalyst, the immobilized enzyme provides an active catalytic center during the reaction process. The amount of input affects the reaction time of the enzyme and is a key factor in product quality and cost.

[0083] In the following, combined with the specific recovery process, the experiment is first carried out on the influence of the dosage of immobilized enzyme.

[0084] (1) Add 1000ml of cefadroxil crystallized mother liquor prepared by the enzymatic cefadroxil process route into the reactor with stirring, the concentration of cefadroxil is about 15mg / ml, heat up to 20°C, control the dosage of EDTA, sulfurous acid Sodium hydrogen 0.80g, adjust the pH of the mother liquor to 7.0 with ammonia water, stir for later use.

[0085] (2) For a self-designed bioreactor, put an appropriate amount of 12.75g to 45g of immobilized biological enzyme into the bioreactor, put it into the feed liquid c...

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 provides a 7-ADCA recovery method, and belongs to the technical field of heterocyclic compounds. The 7-ADCA recovery method comprises the following steps that mother liquor after crystallization of cefadroxil is taken and heated to 10-30 DEG C; the pH value of the mother liquor is adjusted to 7.0-8.0, EDTA is added, and stirring is carried out; an immobilized enzyme is added, the pH value is maintained at 7.0-8.0 and the temperature at 10-30 DEG C, and stirring is carried out until the concentration of the cefadroxil does not exceed 0.5 mg / ml; separating is carried out to remove the immobilized enzyme, the solution obtained by separation is decolored and filtered; the pH value of the filtrate is adjusted to 5.0-6.0, the temperature is controlled to be 10-30 DEG C, and crystals are grown; and filtering and separating are carried out, and a wet product is rinsed to obtain 7-ACDA with the purity of more than 98.5%. The7-ADCA recovery method is green and environment-friendly in technical route, simple to operate, high in yield, stable and reliable, and obvious in advantages.

Description

technical field [0001] The application relates to a 7-ADCA recovery method, which belongs to the technical field of heterocyclic compounds. Background technique [0002] Cefadroxil (cefadroxil) is the first-generation oral cephalosporin, which has a broad antibacterial spectrum and good oral efficacy. Treatment of intestinal infections, etc. The traditional synthesis method mainly uses 7-ADCA (7-aminodesacetoxy cephalosporanic acid) nucleus to carry out acylation condensation of mixed anhydrides of D-hydroxyphenylglycine Deng salt and pivaloyl chloride under cryogenic conditions of liquid nitrogen. , after acid hydrolysis and a large amount of DMF solvent to prepare cefadroxil DMF complex, and then carry out water phase transformation to obtain cefadroxil, the whole process uses a large amount of solvents such as dichloromethane, tetramethylguanidine, DMF, etc., and the reaction conditions are harsh. And the pollution is big. Because adopt twice crystallization, yield is ...

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
IPC IPC(8): C12P35/02
CPCC12P35/02Y02P10/20
Inventor 杜二洪宋迎权郑国荣方金凤徐成苗求满金何丽胡敏
Owner ZHEJIANG ANGLIKANG PHARMA
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
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap