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Separation and purification method for cefaclor by enzymatic synthesis

A cefaclor and enzymatic synthesis technology, applied in organic chemistry, fermentation, etc., can solve the problems of inconvenient batch purification, large amount of solvent usage, harsh reaction conditions, etc., to reduce side chain consumption, increase batch feeding, and stable quality Effect

Active Publication Date: 2014-02-12
苏州盛达药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The shortcoming of cefaclor chemical synthesis method is: 1, will use a large amount of organic solvents in the chemical synthesis process, as dichloromethane, DMF etc.
2. The reaction conditions are relatively harsh, and condensation acylation is generally carried out under cryogenic conditions
3. After the reaction is completed, crystallization in water or the formation of DMF solvate to purify the crystallization, the process consumes a lot of energy, the amount of solvent used is large, and the resulting product contains a lot of impurities
Due to the low solubility of cefaclor in water, and under the condition of enzyme-catalyzed pH value, it cannot form ammonia salt and dissolve in the reaction system, but gradually precipitates out. As the enzyme-catalyzed reaction proceeds, the reaction system will gradually become viscous , making it difficult to control the response
Sometimes it can only be solved by reducing the feeding concentration and increasing the water volume, but the increase in water volume is not suitable for industrial production, and the batch size is too small to bring inconvenience to subsequent purification

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  • Separation and purification method for cefaclor by enzymatic synthesis
  • Separation and purification method for cefaclor by enzymatic synthesis

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Embodiment 1

[0024] Embodiment 1: A kind of separation and purification method of enzymatic synthesis of cefaclor

[0025] In a 1000ml enzyme reactor, add 300ml of water, 25g of 7-amino-3-chlorocephalosporanic acid (7-ACCA), control the temperature at 11~20°C, add ammonia solution dropwise to pH 7.0±0.1, stir to dissolve, add fixed Add 25g of enzyme, and then drop 24g of D-phenylglycine methyl ester hydrochloride solution through the dropping funnel to obtain the enzymatic reaction system, and then use the pH automatic control device to control the pH value of the enzymatic reaction system to be constant at 6.5~6.8. The immobilized enzyme was separated once in 30 minutes and reacted to generate cefaclor. The separation method is to pass the enzymatic reaction solution through a 125-micron sieve, the oversize, that is, the immobilized enzyme, is returned to the enzyme-catalyzed reaction system, and the undersize is filtered to obtain the filtrate and filtrate, and the filtrate is washed and...

Embodiment 2

[0029] Embodiment 2: A kind of separation and purification method of enzymatic synthesis of cefaclor

[0030] In a 1000ml enzyme reactor, add 500ml H 2 O, 30g of 7-ACCA, control the temperature at 18~22℃, add ammonia water dropwise to pH 7.0±0.1, stir to dissolve, add 20g of immobilized enzyme, add 37g of D-phenylglycine methyl ester methanesulfonate solution dropwise through the dropping funnel to obtain Enzyme-catalyzed reaction system, the pH value of the reaction is controlled by the pH automatic control device to be constant at 6.5~6.8, cefaclor is continuously precipitated as the reaction progresses, continuous separation and circulation, the precipitated cefaclor is collected, and the mother liquor is recycled back to the enzyme reactor, 3.5 hours or so. Specifically, the pipeline is connected from the 1000ml enzyme reactor. The pipeline first leads to a screen, a filter device is arranged under the screen, a filtrate collection bucket is arranged under the filter devi...

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Abstract

The invention discloses a separation and purification method for cefaclor by enzymatic synthesis. The separation and purification method comprises the following steps: dissolving 7-ACCA by ammonia water in a water phase, thereafter adding immobilized enzyme; keeping the temperature within 10-35 DEG C; dripping phenylglycine methyl ester hydrochloride or phenylglycine methyl ester mesylate; continuously maintaining the pH value of the reaction within 5.5-7.5; continuously making the generated cefaclor be precipitated from the system with occurrence of enzyme digestion; continuously separating the immobilized enzyme M-1 from the cefaclor by a filtering separation method in an enzymatic liquid; circulating the mother liquid back to a reactor until the 7-ACCA has complete reaction; purifying the obtained wet cefaclor product, and then obtaining the cefaclor. According to the separation and purification method disclosed by the invention, during precipitation of the cefaclor, the cefaclor is separated from the enzymatic reaction liquid, so that the problems of separation and reaction concentration of the enzymic catalytic reaction are solved.

Description

technical field [0001] The present invention relates to a separation and purification method for enzymatically synthesizing cefaclor, in particular to a method for directly biocatalytically synthesizing cefaclor from 7-ACCA, the mother nucleus of cefaclor, and phenylglycine derivatives in water phase through a biological enzymatic method The separation and purification method belongs to the technical field of biomedicine and chemical engineering. Background technique [0002] Cefaclor is the second-generation oral cephalosporin antibiotic studied by Eli Lilly Company in the United States in the early 1980s. Its synthesis method is the earliest by chemical synthesis. The shortcoming of cefaclor chemical synthesis method is: 1, will use a large amount of organic solvents in the chemical synthesis process, as dichloromethane, DMF etc. 2. The reaction conditions are relatively harsh, and condensation acylation is generally carried out under cryogenic conditions. 3. After the r...

Claims

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Application Information

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IPC IPC(8): C12P35/04C07D501/59C07D501/12
Inventor 周自金罗新祖王金龙杨虎星龚仁巍
Owner 苏州盛达药业有限公司
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