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Preparation method for cefotaxime acid

A technology of cefotaxamic acid and 7-ACA, applied in the field of medicine, can solve the problems of multiple separation of intermediates, long synthesis route, complicated operation and the like, and achieves the effects of low price, mild reaction and simple operation

Inactive Publication Date: 2018-09-28
淄博鑫泉医药技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial production process mainly adopts the AE-active ester method, generally using acetone, dichloromethane and tetrahydrofuran as reaction solvents, and reacting with 7-ACA under alkali catalysis, but there are long synthetic routes and multiple separations of intermediates. Problems of complicated operation and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Add 130ml of dichloromethane, 20ml of ethanol and 14ml of triethylamine into the three-necked flask, stir and cool down to 0°C, add 20g of 7-ACA, 26g of MEAM, and react at a temperature of 22°C for 40min;

[0028] 2. After the reaction is completed, add 160ml of purified water and 8ml of triethylamine mixture, control the temperature at 11°C, continue the reaction for 20 minutes, let it stand for 20 minutes, and extract the water phase; add 1g of activated carbon to the water phase, decolorize for 20 minutes, and filter;

[0029] 3. After the decolorization is completed, add 60ml of ethanol, control the temperature at 18°C, use 140g of dilute hydrochloric acid with a concentration of 10wt.% to crystallize, adjust the pH value to 2.8, cool down to 3°C, and grow crystals for 30 minutes; filter with suction and use 80ml of purified water Wash with 100ml of acetone and dry at 55°C to obtain 32.10g of dry cefotaxime acid; yield 1.605, content 95.12%, simple impurities 0.25...

Embodiment 2

[0031] 1. Add 185ml of dichloromethane, 31ml of ethanol and 20ml of triethylamine into the three-necked flask, stir and cool down to 0°C, add 30g of 7-ACA, 39g of MEAM, and react at 23°C for 45min;

[0032] 2. After the reaction is completed, add 255ml of purified water and 9g of sodium bicarbonate mixture, control the temperature at 12°C, continue the reaction for 20 minutes, let it stand for 20 minutes, and extract the water phase; add 1.2g of activated carbon to the water phase, decolorize for 20 minutes, and filter;

[0033] 3. After the decolorization is completed, add 114ml of ethanol, control the temperature at 16°C, use 120g of dilute hydrochloric acid with a concentration of 15wt.% to crystallize, adjust the pH value to 2.6, lower the temperature to 4°C, and grow the crystal for 30 minutes; filter with suction and use 120ml of purified water , 120ml of acetone washing material, drying at 58°C to obtain 32.18g dry product of cefotaxime acid; yield 1.609, content 95.21%,...

Embodiment 3

[0035] 1. Add 277ml of dichloromethane, 37ml of ethanol and 28ml of triethylamine into the three-necked flask, stir and cool down to 0°C, add 40g of 7-ACA, 48g of MEAM, and react at a temperature of 22°C for 50 minutes;

[0036] 2. After the reaction is completed, add 340ml of purified water and 12g of 10% ammonia water mixture, control the temperature at 13°C, continue the reaction for 20 minutes, let it stand for 20 minutes, and extract the water phase; add 1.6g of activated carbon to the water phase, decolorize for 20 minutes, and filter;

[0037] 3. After the decolorization is completed, add 127ml of isopropanol, control the temperature at 19°C, crystallize with 110g of dilute hydrochloric acid with a concentration of 20wt.%, adjust the pH value to 2.4, cool down to 2°C, and grow crystals for 30 minutes; filter with suction and purify with 240ml Wash the material with water and 203ml of acetone, and dry it at 60°C to obtain 32.22g of dry cefotaxime acid; the yield is 1.611,...

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Abstract

The invention relates to a preparation method for cefotaxime acid, belonging to the technical field of medicines. The preparation method for the cefotaxime acid comprises the following steps: preparation of a condensed liquid: a step of adding 7-ACA and MEAM into a mixed solvent of dichloromethane, ethanol and triethylamine, and carrying out a reaction for 30 to 60 min; extraction and decolorization: a step of extracting the prepared condensed liquid with purified water and an alkali mixed solution so as to obtain an aqueous phase, and adding active carbon into the aqueous phase for decolorization; and preparation of a finished product: a step of adding monohydric alcohol after decolorization is completed, carrying out crystallization with diluted hydrochloric acid, adjusting the pH valueof a solution to 2.0 to 3.0, carrying out cooling, allowing a crystal to grow, carrying out vacuum filtering, washing an obtained material with the purified water and acetone, and carrying out dryingso as to obtain a dry cefotaxime acid product. The preparation method for the cefotaxime acid provided by the invention is scientific, reasonable, simple and practicable; and the cefotaxime acid obtained by using the preparation method provided by the invention has low impurity content and high yield.

Description

technical field [0001] The invention relates to a preparation method of cefotaxime acid, which belongs to the technical field of medicine. Background technique [0002] Cefotaxime sodium is a third-generation cephalosporin antibiotic widely used clinically. The drug was jointly developed by Hoechst of Germany and Roussel of France in 1977, and was launched in 1980. It has broad-spectrum, high efficiency, enzyme resistance, toxicity The characteristics of small side effects. It is mainly used for respiratory system infection, biliary tract and intestinal infection, skin and soft tissue infection, burn and bone and joint infection caused by sensitive bacteria. Cefotaxime acid is the main raw material for preparing cefotaxime sodium. With the increasingly fierce market competition, it is of practical significance to study its synthesis process, reduce production costs and improve product quality. [0003] The synthesis of cefotaxime acid mainly adopts active ester method: suc...

Claims

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Application Information

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IPC IPC(8): C07D501/06C07D501/34
CPCC07D501/06C07D501/34
Inventor 张立明尹纪松周红艳
Owner 淄博鑫泉医药技术服务有限公司
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