Preparation of cefixime cephalosporin and fine purification method

A technology of cefixime and a refining method, applied in the field of oral cephalosporins, can solve the problems of low reaction process stability, uneven product quality, inconvenient industrialized production, etc., and achieve considerable economic benefits, good product quality and convenience The effect of industrial production

Inactive Publication Date: 2008-07-16
四川方向海瑞实业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although there are many reports on the preparation methods of cefixime at present, these methods usually have the disadvantages of long preparation time, high requirements for equipment, low reaction process stability and uneven product quality, which have brought great challenges to industrialized production. the inconvenience

Method used

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  • Preparation of cefixime cephalosporin and fine purification method
  • Preparation of cefixime cephalosporin and fine purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 500ml dry three-necked flask, add 150ml of ethanol, lower the temperature to below 0°C, add 20g of cefixime methyl triethylamine salt under stirring, add 20ml of anhydrous formic acid, stir for 2 hours, and drop 98% of Sulfuric acid 8ml, stirred for 3 hours, filtered, washed with ethanol, and dried in vacuum at 50°C to obtain cefixime monohydrate monosulfate 13.6g. (Yield: 82%)

[0021] In a 1000ml three-necked flask, add 150ml of deionized water, lower the temperature to below 0°C, add 13.6g of cefixime monosulfate monohydrate under constant stirring, adjust the pH value to 5.5 with ammonia water, add 1g of activated carbon, decolorize and filter, and add 1g of activated carbon to the filtrate Add 100ml of ethanol, use 4mol / L hydrochloric acid to adjust the pH value to 4, raise the temperature to 25°C, then use 4mol / L hydrochloric acid to adjust the pH value to 2.5, stir for 30 minutes and then drop to below 0°C, stir for 2 hours, filter, Washed with ice water an...

Embodiment 2

[0023] In a 500ml dry three-necked flask, add 150ml of acetone, lower the temperature to below 0°C, add 20g of cefixime methyl triethylamine salt under stirring, add 20ml of anhydrous formic acid, stir for 2 hours, and drop 98% of Sulfuric acid 8ml was stirred for 3 hours, filtered, washed with acetone, and dried in vacuum at 50°C to obtain cefixime monohydrate monosulfate 13.1g. (Yield: 79%)

[0024] In a 1000ml three-neck flask, add 150ml of deionized water, lower the temperature to below 0°C, add 13.1g of cefixime monohydrate monosulfate under constant stirring, adjust the pH value to 7.5 with ammonia water, add 1g of activated carbon, decolorize and filter, and add to the filtrate Add 100ml of ethanol, use 4mol / L hydrochloric acid to adjust the pH value to 4, raise the temperature to 25°C, then use 4mol / L hydrochloric acid to adjust the pH value to 2.62, stir for 30 minutes, then drop to below 0°C, stir for 2 hours, filter, Washed with ice water and dried under vacuum at ...

Embodiment 3

[0026] In a 500ml dry three-necked flask, add 150ml of methanol, lower the temperature to below 0°C, add 20g of cefixime methyl triethylamine salt under stirring, add 20ml of anhydrous formic acid, stir for 2 hours, and drop 98% of Sulfuric acid 8ml, stirred for 3 hours, filtered, washed with methanol, and vacuum-dried at 50°C to obtain cefixime monohydrate monosulfate 12.8g. (Yield: 77.2%)

[0027] In a 1000ml three-neck flask, add 150ml of deionized water, lower the temperature to below 0°C, add 12.8g of cefixime monohydrate monosulfate under constant stirring, adjust the pH value to 5.9 with ammonia water, add 1g of activated carbon, decolorize and filter, and add to the filtrate Add 100ml of ethanol, use 4mol / L hydrochloric acid to adjust the pH value to 4, raise the temperature to 25°C, then use 4mol / L hydrochloric acid to adjust the pH value to 2.5, stir for 30 minutes and then drop to below 0°C, stir for 2 hours, filter, Washed with ice water and dried under vacuum at ...

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Abstract

The invention relates to a preparation and refining method for cefixime, which is conducted as in the following technical steps: the first step, cefixime methyl triethyl amine salt is dissolved in an organic solvent, filtered and washed after reaction with formic acid anhydrous and 98 percent of concentrated sulfuric acid below 0 DEG C, and dried in vacuum at 50 DEG C to obtain cefixime monohydrate monosulphate; the second step, the cefixime monohydrate monosulphate is dissolved in deionized water below 0 DEG C, the pH value is adjusted by ammonia, after being discolored and filtrated by activated carbon, the filtrate is added with ethanol and then 4mol / L of hydrochloride is used for adjusting the pH value, and after filtering, washing by icing water and drying at 30 DEG C in vacuum, cefixime trihydrate acid products are obtained. The method has the advantages of simple operation, little pollution, low manufacturing cost, good quality of prepared cefixime, great convenience for industrialization manufacturing and substantial economic benefits. Simultaneously, as the product of cefixime is presented as white powder with content over 98 percent, guarantees are provided for safe medication in the quality of medicines.

Description

technical field [0001] The present invention relates to an oral cephalosporin, specifically, the present invention relates to cefixime, namely (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2- (Carboxymethoxyimino)]acetamido]-8-oxo-3-ethylene-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid trihydrate and the preparation and purification method of the compound. Background technique [0002] Cefixime is the third-generation oral cephalosporin, which plays a bactericidal effect by inhibiting the synthesis of bacterial cell walls. It is stable to most β-lactamases. Many strains producing penicillinase and cephalosporinase are still sensitive to this product. Cefixime is effective against Gram-positive cocci such as pneumococcus and Streptococcus pyogenes in vitro and in vivo, Gram-negative bacilli such as influenza bacilli (including enzyme-producing strains), Moraxella catarrhalis (including enzyme-producing strains), large intestine Bacillus, Proteus mirabilis, and Neisseria ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22
Inventor 朱晓茂余安国林国华莫兆明
Owner 四川方向海瑞实业有限责任公司
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