Reworking method of cefpirome sulfate

A technology of cefpirome sulfate and filtrate, which is applied in the field of rework of cefpirome sulfate, can solve the problems of waste, complex synthetic route, expensive price, etc., and achieve the effect of cost reduction

Inactive Publication Date: 2013-04-17
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Cefpirome sulfate is the fourth generation of broad-spectrum cephalosporin antibiotics. It has the characteristics of broad-spectrum and high-efficiency inhibition of β-lactamase. It is clinically used for the treatment of patients with moderate and severe infections. Its syn

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 20g of cefpirome sulfate to be reworked in 120ml of water, add triethylamine dropwise to dissolve, adjust the pH value to 6.0-6.5, pass the dissolved solution through a γ-alumina column, collect 160ml of filtrate, add 1g of activated carbon for decolorization After 30 minutes, filter, adjust the pH of the filtrate to the optimum value of pH 1.6 to 2.0 with sulfuric acid solution, add a certain amount of acetone to crystallize, control the reaction temperature during crystallization at 18°C ​​to 22°C, and stir for 2 to 4 hours to end the reaction and filter , washed with acetone mixed solution, vacuum-dried at 45-55° C. until the water content is qualified, to obtain 17.5 g of cefpirome sulfate, and the recovery rate of cefpirome sulfate to be reworked can reach 87.5%.

Embodiment 2

[0033] Dissolve 20g of cefpirome sulfate to be reworked in 120ml of water, add ammonia water dropwise to dissolve, adjust the pH value to 6.0-6.5, pass the dissolved solution through a γ-alumina column, collect 160ml of filtrate, add 1g of activated carbon for decolorization for 30min, Filtrate, adjust the pH of the filtrate to the optimum pH value of 1.6~2.0 with sulfuric acid solution, add a certain amount of alcohol for crystallization, control the reaction temperature during crystallization at 18°C~22°C, and stir for 2~4h, end the reaction, filter, acetone The mixture was washed, and vacuum-dried at 45-55° C. until the moisture content was qualified to obtain 18.0 g of cefpirome sulfate. The recovery rate of the cefpirome sulfate to be reworked could reach 90.0%.

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Abstract

The invention discloses a reworking method of cefpirome sulfate. The reworking method comprises the following steps of: 1) dissolving the cefpirome sulfate to be reworked in a certain amount of water; 2) dripping an organic base for dissolution, regulating the PH value to 4.0-8.0, and setting the reaction temperature at 0 DEG C-30 DEG C; 3) enabling the solution after dissolution to pass through a column loaded with an adsorbent, and collecting filtrate; 4) adding activated carbon into the filtrate, performing decolorization reaction for 30min, and filtering; 5) regulating the PH value of the filtrate after decolorization to 1.2-2.4; 6) adding a quantitative crystallizing agent into the filtrate for crystallization, controlling the crystallization temperature at 0 DEG C-30 DEG C, and stirring for 2-4h till the end of reaction; 7) filtering, and washing with one solution or a mixed solution of acetone and alcohol; and 8) drying at the temperature of 45 DEG C-55 DEG C to obtain the cefpirome sulfate. According to the reworking method disclosed by the invention, the unqualified cefpirome sulfate can be effectively reworked and refined to produce a qualified product, and the cost can be further reduced.

Description

technical field [0001] The invention relates to a reworking method of cefpirome sulfate. Background technique [0002] Cefpirome sulfate is the fourth generation of broad-spectrum cephalosporin antibiotics. It has the characteristics of broad-spectrum and high-efficiency inhibition of β-lactamase. It is clinically used for the treatment of patients with moderate and severe infections. Its synthetic route is relatively complicated and expensive. Unqualified color, content, impurity, sterility, visible foreign matter, etc. may sometimes occur due to other reasons in the preparation process, and the unqualified cefpirome sulfate is discarded, which is relatively wasteful. Contents of the invention [0003] For overcoming above-mentioned shortcoming, the object of the present invention is to provide a kind of reworking method that can effectively refine unqualified cefpirome sulfate into qualified product, and the rework method of the cefpirome sulfate of cost reduction. [0...

Claims

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Application Information

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IPC IPC(8): C07D501/46C07D501/12
Inventor 周自金曾润保冷雄军温雄飞吕德新
Owner 苏州盛达药业有限公司
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