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Process for preparing cefixime

A technology for cefixime and cefixime methyl ester, which is applied in the field of preparation of cefixime, can solve the problems of inability to recover mercaptobenzothiazole well, the use of deprotection agents is toxic, and the production cost is low, and achieves hydrolysis and crystallization. And the effect of improving the quality of finished products, reducing production costs and improving product quality

Active Publication Date: 2008-12-10
ZHEJIANG ANGLIKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the existing defects of the above-mentioned existing cefixime preparation method, the main purpose of the present invention is to provide a kind of cefixime preparation method, which solves the problem that mercaptobenzothiazole cannot be well recovered in the original process, and improves the yield of the product. rate and finished product quality
[0010] A further object of the present invention is to provide a preparation method of cefixime, which solves the problem of using toxic and expensive trifluoroacetic acid as a deprotection agent in the original process, and has the advantages of low production cost and good environmental protection

Method used

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  • Process for preparing cefixime

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Put DMF / 22.5ml, methylene chloride 83ml into a 500ml three-necked flask, add 4.7g sodium iodide, 8.9g triphenylphosphine, 15g GCLE, heat up to 30°C for 1 hour, cool down to 10°C, add formaldehyde 27 gram, 100ml of 8% liquid caustic soda, react for 10 minutes, adjust the pH value to 4 with hydrochloric acid, add water and dichloromethane to dilute the system, separate the water layer, recover the dichloromethane layer to dryness, add methanol, heat up to 40 degrees to crystallize , After adding water, cool to 3 degrees, and filter to get GVNE. Put 50 grams of phenol into a three-necked flask, raise the temperature to 100 degrees to activate for two hours, then add dry GVNE / 25 grams, react for 10 hours until the GVNE residue is qualified, add butyl acetate and water, separate the water layer, and use butyl acetate again Wash the water layer with ester, add activated carbon to decolorize and filter the water layer after layering, add 25 grams of enzyme to the filtrate, rai...

Embodiment 2

[0049] The preparation method and process are the same as in Example 1, except that ethylene glycol is used to prepare cefixime methyl.

Embodiment 3

[0051] Put DMF / 22.5ml, methylene chloride 83ml into a 500ml three-necked flask, add 4.7g sodium iodide, 8.9g triphenylphosphine, 15g GCLE, heat up to 30°C for 1 hour, cool down to 10°C, add formaldehyde 27 gram, 100ml of 8% liquid caustic soda, react for 10 minutes, adjust the pH value to 4 with hydrochloric acid, add water and dichloromethane to dilute the system, separate the water layer, recover the dichloromethane layer to dryness, add methanol, heat up to 40 degrees to crystallize , After adding water, cool to 3 degrees, and filter to get GVNE. Put 50 grams of phenol into a three-necked flask, raise the temperature to 100 degrees to activate for two hours, then add dry GVNE / 25 grams, react for 10 hours until the GVNE residue is qualified, add butyl acetate and water, separate the water layer, and use butyl acetate again Wash the water layer with ester, add activated carbon to decolorize and filter the water layer after layering, add 25 grams of enzyme to the filtrate, rai...

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Abstract

The invention provides a method for preparing cefixime, which belongs to the medicine synthesis technical field and comprises the steps of preparation of 7-AVCA, preparation of cefixime methyl ester, preparation of the cefixime and so on. The method aims at the prior amino de-protection to make an improvement, and uses penicillin acylase to substitute trifluoroacetic acid and so on in the prior process to ensure that an amino de-protection reaction is greatly improved, the use of organic solvents can be completely avoided, and acylase can also be reused at the same time. Methylene dichloride and tetrahydrofuran solvents in the prior process are substituted by adopting alcohol, ketone or ester solvents, so that an amidation reaction is greatly improved, which ensures that reaction solvents are easy to recover and reuse, can reduce production cost, reduce the discharge of waste liquid, reduce the pollution to the environment, can completely recover a byproduct, namely mercaptobenzothiazole produced by the reaction, improve the atom utilization rate of reaction raw-materials, and greatly improve the hydrolyzation and crystallization of subsequent products and the quality of a finished product.

Description

technical field [0001] The invention relates to a preparation method of cefixime, which belongs to the technical field of cefixime synthesis in the chemical pharmaceutical industry. Background technique [0002] Cefixime is a third-generation oral cephalosporin antibiotic, which has a broad-spectrum antibacterial effect on Gram-positive and negative bacteria, especially against influenza, pneumococcus and Gram-positive bacteria. Among the negative bacteria, Escherichia coli, Moraxella, Neisseria gonorrhoeae, Proteus mirabilis, Cathaeria, etc. showed stronger bactericidal effect than other oral cephalosporins. It has the characteristics of broad spectrum, high efficiency, drug resistance, and low toxicity, and is an anti-infective oral drug widely used in clinical practice. [0003] The preparation method of cefixime is mainly as follows at present: [0004] 1. Preparation of cefixime intermediate 7-AVCA: using GCLE as raw material, GCLE first reacts with sodium iodide and ...

Claims

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Application Information

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IPC IPC(8): C12P35/04
Inventor 程先波胡立蓬叶树祥徐成苗马海岭
Owner ZHEJIANG ANGLIKANG PHARMA
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