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Method for preparing cefotaxime acid

A technology of cefotaxime acid and carboxylic acid, which is applied in the field of preparation of cefotaxime acid, can solve the problems of low content of cefotaxime acid, achieve the effect of shortening the reaction time, increasing the content and conversion rate

Active Publication Date: 2014-09-10
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is exactly to provide a kind of new preparation method of cefotaxime acid, to solve the problem that the cefotaxime acid content that existing preparation method makes is on the low side problem

Method used

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  • Method for preparing cefotaxime acid
  • Method for preparing cefotaxime acid
  • Method for preparing cefotaxime acid

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Mix 20.0 g of 7-ACA and 26.0 g of AE-active ester in 130 ml of dichloromethane and 20 ml of isopropanol, add 1 g of tetrabutylammonium bromide and 14 ml of triethylamine, and react with water for 1 h. Extract the organic phase twice, adjust the pH to 2.5-3.0 with hydrochloric acid, crystallize at room temperature for 1 h, and filter with suction to obtain 37 g of cefotaxime acid wet powder. Add 740 ml of acetone, heat, and reflux for 30 at a temperature of 30°C. Min, cool to 0°C, filter, and dry for 5 h at a temperature of 40°C to obtain 33.03 g of cefotaxime acid.

Embodiment 2

[0025] Mix 20.0 g of 7-ACA and 26.0 g of AE-active ester in 138.7 ml of dichloromethane and 21.3 ml of isopropanol, add 0.02 g of tetrabutylammonium bromide and 17 ml of triethylamine, and react with water for 1 h. Extract the organic phase twice, adjust the pH to 2.5-3.0 with hydrochloric acid, crystallize at room temperature for 1 h, and filter with suction to obtain 37 g of cefotaxime acid wet powder, add 111 ml of acetone, heat, and reflux at 30°C for 30 min. The temperature was lowered to 0°C, filtered, and dried at a temperature of 50°C for 4 hours to obtain 33.06 g of cefotaxime acid.

Embodiment 3

[0027] Mix 20.0 g of 7-ACA and 26.0 g of AE-active ester in 140 ml of dichloromethane and 20 ml of methanol, add 0.1 g of tetrabutylammonium chloride and 18 ml of triethylamine, and extract twice with water after reacting for 1 hour. For the organic phase, adjust the pH to 2.5-3.0 with hydrochloric acid, crystallize at room temperature for 1 h, and filter to obtain 37 g of cefotaxime acid wet powder, add 370 ml of acetone, heat, reflux for 30 min at a temperature of 30℃, and cool down To 0°C, filter, and dry for 3 h at a temperature of 65°C to obtain 33.04 g of cefotaxime acid.

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Abstract

The invention discloses a method for preparing cefotaxime acid, which comprises the steps as follows: (a) 7-ACA and AE-active ester are weighed according to mass ratio that is 1:1.3, are mixed, and then are dissolved in a mixed solvent formed by methylene dichloride and a latent solvent, and stirring is carried out so as to obtain mixed solution; (b) triethylamine and a phase-transfer catalyst are sequentially added in the mixed solution, and reaction is performed for 1 to 2.5 hours under the catalytic action of the phase-transfer catalyst at the room temperature; (c) liquid reactant is extracted through water, hydrochloric acid is added in aqueous extract to regulate the pH value, and crystallization and filtration are carried out, so as to obtain wet cefotaxime acid powders; and (d) the wet powder is dissolved in organic solvent, and heating backflow, temperature reduction, filtration and drying are carried out, so as to obtain cefotaxime acid. The method with simple technology is convenient to operate; the obtained cefotaxime acid achieves high content, high yield coefficient and low moisture content, can be used as a main raw material of cynnematin-cefotaxime sodium, and can achieve an anti-inflammatory bactericidal effect and the like on pneumonia, respiratory tract infection, urinary tract infection, meningitis, skin and soft tissue infection and the like caused by susceptible bacteria.

Description

Technical field [0001] The invention relates to a method for preparing a cephalosporin medicine, in particular to a method for preparing cefotaxime acid. Background technique [0002] Cefotaxime, scientific name (6R, 7R)-3-[(acetoxy)methyl]-7-[(2-amino-4-thiazolyl)-(methoxyimino)acetamido] -8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, a third-generation cephalosporin antibiotic, can be used as cephalosporin-cefotaxel for injection The main raw material of sodium oxime is used for pneumonia and respiratory infections, urinary tract infections, meningitis, sepsis, abdominal infections, pelvic infections, skin and soft tissue infections, reproductive tract infections, bone and joint infections, which have anti-inflammatory and sterilizing effects. At present, there are many preparation processes for cefotaxime acid, including phosphorus-containing active ester method, triazone active ester method, oxadiazole active ester method and AE active ester method. Among them...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/34C07D501/06
Inventor 张军立刘倩王玉红姚宝林高俊艳
Owner NORTH CHINA PHARMA COMPANY
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