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Cefprozi compound and preparation method thereof

A technology of cefprozil and its compounds, which is applied in the field of medicine, can solve the problems of low purity of cefprozil, and achieve the effects of low cost, convenient operation and quality improvement

Inactive Publication Date: 2010-11-10
郑仙锋
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortcoming of low purity of cefprozil prepared in the prior art, provide a method for refining cefprozil compound, fundamentally greatly improve the purity of cefprozil, and ensure the quality of the preparation

Method used

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  • Cefprozi compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Get cefprozil crude product 100g, add the potassium hydroxide solution of 1mol / L, adjust pH value to 10, fully react to clarification, obtain cefprozil potassium solution, then through Hz816 adsorption resin adsorption, after adsorption is complete, use volume ratio as 1: 1 isopropanol-water mixture to elute cefprozil potassium salt, collect the eluent, add 6g of activated carbon for adsorption for 30 minutes, filter for decarburization, add 2mol / L hydrochloric acid solution to the filtrate, adjust the pH value to 2, precipitate crystals, and filter , washed with water, and dried under reduced pressure at 50° C. to obtain 91.1 g of cefprozil crystals, with a yield of 91.1%, and a purity of 99.7% as detected by HPLC.

Embodiment 2

[0019] Get cefprozil crude product 100g, add the sodium hydroxide solution of 4mol / L, adjust pH value to 7, fully react to clarification, obtain cefprozil sodium solution, then through AmberliteXAD-4 adsorption resin adsorption, after adsorption is complete, with volume ratio: 1:1 acetonitrile-water mixture to elute cefprozil sodium salt, collect the eluate, add 4g activated carbon for 20 minutes, filter for decarburization, add 5mol / L acetic acid solution to the filtrate, adjust the pH value to 5, precipitate crystals, filter , washed with water, and dried under reduced pressure at 40° C. to obtain 92.4 g of cefprozil crystals, with a yield of 87.8%, and a purity of 99.9% as detected by HPLC.

Embodiment 3

[0021] Get cefprozil crude product 100g, add 10% potassium bicarbonate solution, adjust the pH value to 8.5, fully react to clarification, obtain cefprozil potassium solution, then through AmberliteXAD-4 adsorption resin adsorption, after adsorption is complete, use a volume ratio of 3 : 1 ethanol-water mixture to elute cefprozil sodium salt, collect the eluent, add 5g of active carbon for adsorption for 30 minutes, filter for decarburization, add 2mol / L nitric acid solution to the filtrate, adjust the pH value to 3.5, precipitate crystals, filter, After washing with water and drying under reduced pressure at 45°C, 93.1 g of cefprozil crystals were obtained, with a yield of 93.1%, and a purity of 99.5% by HPLC.

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Abstract

The invention relates to a cefprozi compound and a preparation method thereof. The method prepares a comparatively pure cefprozi compound from a cefprozi crude product prepared by the prior art through the following steps of: adding alkaline solution into the cefprozi crude product and adjusting the pH value to perform full reaction until the mixture is clarified, or dissolving cefprozi into an organic solvent, and adding the alkaline solution for reaction to obtain cefprozi saline solution; performing adsorption by using macroporous polymeric adsorbent; after complete adsorption, eluting a cefprozi salt by using an eluant; collecting elutriant; adding active carbon into the elutriant for adsorption; filtering the elutriant; adding filtrate into acidic solution; adjusting the pH value; separating out crystals; and filtering, eluting and drying the crystals to obtain cefprozi crystals.

Description

technical field [0001] The invention relates to a method for refining antibiotic drugs, in particular to a method for refining cefprozil compounds, and belongs to the technical field of medicine. Background technique [0002] Cefprozil, its chemical name is: (6R,7R)-7-L(R)-2-amino-2-(p-hydroxyphenyl)acetamido 1-8-oxo-3-propene-5-mercapto -1-azabicyclo-(4.2.0)oct-2-ene-2-carboxylic acid monohydrate, molecular formula: C 18 h 21 N 3 o 6 S, molecular weight: 407.45, structural formula: [0003] [0004] It is a second-generation broad-spectrum cephalosporin antimicrobial drug developed by Bristol-Myers Squibb. + , G - Bacteria and anaerobic bacteria have strong antibacterial activity against G + Bacterial activity is particularly prominent. [0005] At present, the synthetic method of cefprozil mostly adopts GCLE, GCLH route, all have reports in U.S. Patent US4694079, Chinese Patent CN101024649, Chinese Journal of Pharmaceutical Industry. The price of GCLH raw mater...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/12A61P31/00
Inventor 郑仙锋
Owner 郑仙锋