Preparation method of cefaclor suitable for industrial production

A technology of cefaclor and cephalosporin, which is applied in the field of preparation of cefaclor, can solve the problems such as poor effect of enzyme filtration, achieve the effects of reducing production cost and environmental protection expenditure, reducing pressure, and reducing degradation caused by excessive enzyme filtration time

Inactive Publication Date: 2019-01-25
QILU ANTIBIOTICS PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problem of poor enzyme filtering effect in the existing process, the present invention provides a method for preparing

Method used

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  • Preparation method of cefaclor suitable for industrial production
  • Preparation method of cefaclor suitable for industrial production
  • Preparation method of cefaclor suitable for industrial production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 150g of purified water and 40g of 7-ACCA to the clean reaction flask, cool down to 0-5°C, and slowly add 10% sodium hydroxide solution until the solution is clear. Add 45g of immobilized penicillin acylase for synthesis, control the temperature at 5-15°C, add the pre-prepared 40g of PGM solution for about 1 hour, and maintain the pH of the reaction feed solution with sodium bicarbonate solution = 6.0-7.5. After adding PGM, the reaction reaches 7- ACCA residues meet the requirements.

[0046] After the reaction is qualified, use sodium hydroxide to adjust the pH of the reaction feed liquid to 8.0, the feed liquid is dissolved, pour the feed liquid into a specific device, and pass through an 80-mesh filter for separation under stirring. Cool the feed solution to 0-5°C, add activated carbon for decolorization for 30 minutes, filter, wash with purified water, and combine the filtrate and washing liquid into a crystallization bottle.

[0047] Slowly add hydrochloric aci...

Embodiment 2

[0049] Add 150g of purified water and 40g of 7-ACCA to the clean reaction flask, cool down to 0-5°C, and slowly add 10% sodium hydroxide solution until the solution is clear. Add 42g of immobilized penicillin acylase for synthesis, control the temperature at 5-15°C, and add 36.5g of the pre-prepared PGM solution for about 2 hours. The sodium bicarbonate solution maintains the pH of the reaction feed solution at 6.0-7.5, and the reaction reaches 7 after adding PGM. - ACCA residues are compliant.

[0050] After the reaction is qualified, use sodium hydroxide to adjust the pH of the reaction feed liquid to 8.5, the feed liquid is dissolved, pour the feed liquid into a specific device, and pass through an 80-mesh filter for separation under stirring. Cool the feed solution to 0-5°C, add activated carbon for decolorization for 30 minutes, filter, wash with purified water, and combine the filtrate and washing liquid into a crystallization bottle.

[0051]Hydrochloric acid solution ...

Embodiment 3

[0055] Add 150g of purified water and 40g of 7-ACCA to the clean reaction flask, cool down to 0-5°C, and slowly add 10% sodium hydroxide solution until the solution is clear. Add 45g of immobilized penicillin acylase for synthesis, control the temperature at 5-15°C, and slowly add the pre-prepared 41.2g PGM solution for about 3 hours, and the sodium bicarbonate solution to maintain the pH of the reaction feed solution = 6.0-7.5, and react to 7-ACCA residues meet the requirements.

[0056] After the reaction is qualified, use sodium hydroxide to adjust the pH of the reaction feed liquid to 9.0, the feed liquid is dissolved, pour the feed liquid into a specific device, and pass through an 80-mesh filter for separation under stirring. Cool the feed solution to 0-5°C, add activated carbon for decolorization for 30 minutes, filter, wash with purified water, and combine the filtrate and washing liquid into a crystallization bottle.

[0057] Add 0.2 g of seed crystals to the hydroch...

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Abstract

The invention belongs to the technical field of pharmaceutical synthesis and relates to a preparation method of cefaclor suitable for industrial production. The preparation method uses 7 amino-3-chloro-cephem acid as a starting material, and reacts with L-phenylglycine methyl ester hydrochloride under the action of an immobilized penicillin acylase for synthesis to obtain cefaclor. The invention solves the difficult problem of filtering enzyme in the prior art, reduces the production man-hour, has high product yield, produces less three wastes, is green and environmentally friendly, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of cefaclor and belongs to the technical field of drug synthesis. Background technique [0002] Cefaclor [(formula Ⅰ) chemical name is 7-(D-α-phenylglycylamino)-3-chloro-3-cephalosporin-4-carboxylic acid] belongs to the second-generation cephalosporin products, produced by the United States Developed by Eli Lilly and Company, it is one of the best-selling antibiotics in the world. At present, the domestic and foreign production process routes of cefaclor can be divided into chemical method and biological method, both of which use 7-amino-3-chlorocephalosporin (7-ACCA) as the starting material. [0003] [0004] The chemical method is to carry out condensation reaction between 7-ACCA and phenylglycine (need to protect the amino group) in organic solvents such as tetrahydrofuran or acetonitrile, and then use DMF, 2-naphthol and other solvents to form a mixture to purify cefaclor to obtain cephalosporin C...

Claims

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Application Information

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IPC IPC(8): C12P35/04C07D501/59C07D501/12
CPCC07D501/12C07D501/59C12P35/04
Inventor 侯传山刘军浩史韶华王欣范美菊高阳王立
Owner QILU ANTIBIOTICS PHARMA
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