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Synthesis method of cefminox sodium

A technology of cefminox sodium and a synthesis method, which is applied in the field of preparation of cefminox, can solve the problems of complex synthesis operation process, unguaranteed safety, endangering the health of operators, etc., and achieves improved product quality and yield, Ease of control and low energy consumption for production

Inactive Publication Date: 2014-10-01
GUANGDONG LIGUO PHARMACY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic operation process of this method is complex, and after repeated extractions, the yield of the final product is low, and a large amount of organic solvents are used, which seriously pollutes the environment, and also endangers the health of the operator, and the safety cannot be guaranteed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 30g of methicillin (7-MAC) and 180ml of dichloromethane to the reaction bottle ①, add 40.5ml of pyridine and 25.0ml of carbon tetrachloride after the dissolution is complete, and stir the reaction for 50 minutes under temperature control below 15°C; the reaction is completed Finally, add saturated aqueous sodium chloride solution, stir, extract and separate layers, and keep the lower organic phase; add 2.0 g of activated carbon for decolorization, and after filtration, vacuum concentrate the solution until the volume is reduced by 50%; take another reaction bottle ② and add dichloromethane and Ethanol, add 3.2g of hydrogen chloride gas, after completion, add the concentrated solution into the reaction bottle ②, stir and react for 60 minutes at a temperature controlled within 20°C, after the reaction is completed, add 250mL of mixed solvent (ethanol:water=2:1), stir and extract , keep the lower organic phase; add 1.5g activated carbon for decolorization, filter, use 5...

Embodiment 2

[0031] Add 30g of methicillin (7-MAC) and 180ml of dichloromethane to the reaction bottle ①, add 40.5ml of pyridine and 25.0ml of carbon tetrachloride after the dissolution is complete, and stir the reaction for 50 minutes under temperature control below 15°C; the reaction is completed Finally, add saturated aqueous sodium chloride solution, stir, extract and separate layers, and keep the lower organic phase; add 2.0 g of activated carbon for decolorization, and after filtration, vacuum concentrate the solution until the volume is reduced by 50%; take another reaction bottle ② and add dichloromethane and Ethanol, add 3.2g of hydrogen chloride gas, after completion, add the concentrated solution into the reaction bottle ②, stir and react for 60 minutes at a temperature controlled within 20°C, after the reaction is completed, add 250mL of mixed solvent (ethanol:water=2:1), stir and extract , keep the lower organic phase; add 1.5g activated carbon for decolorization, filter, use 5...

Embodiment 3

[0033] Add 30g of methicillin (7-MAC) and 180ml of dichloromethane to the reaction bottle ①, add 40.5ml of pyridine and 25.0ml of carbon tetrachloride after the dissolution is complete, and stir the reaction for 50 minutes under temperature control below 15°C; the reaction is completed Finally, add saturated aqueous sodium chloride solution, stir, extract and separate layers, and keep the lower organic phase; add 2.0 g of activated carbon for decolorization, and after filtration, vacuum concentrate the solution until the volume is reduced by 50%; take another reaction bottle ② and add dichloromethane and Ethanol, add 3.2g of hydrogen chloride gas, after completion, add the concentrated solution into the reaction bottle ②, stir and react for 60 minutes at a temperature controlled within 20°C, after the reaction is completed, add 250mL of mixed solvent (ethanol:water=2:1), stir and extract , keep the lower organic phase; add 1.5g activated carbon for decolorization, filter, use 5...

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Abstract

The invention discloses a synthesis method of cefminox sodium, which comprises the following steps: completely dissolving methoxycephalosporin (7-MAC) and dichloromethane in a reaction flask (1), and adding pyridine and carbon tetrachloride; after complete reaction, adding a saturated aqueous solution of sodium chloride for extracting and layering, and performing vacuum concentration on a bottom-phase organic phase; adding dichloromethane and ethanol into a reaction flask (2), and introducing hydrogen chloride gas; after complete reaction, adding the concentrated liquid in the reaction flask (1) into the reaction flask (2); after complete reaction, adding a mixed solvent for extracting and layering; performing liquid separation on the organic phase by use of the saturated aqueous solution of sodium chloride, and keeping the bottom-phase organic phase; adding D-cysteine into the organic phase, adjusting the pH value of the solution to 6.0-6.5, and keeping the temperature at 20-25 DEG C; after sufficient reaction, feeding ethanol, and performing sufficient crystal precipitation and vacuum drying to obtain cefminox sodium. According to the method, the reaction process causes low toxicity, the operation is safe, the quality and yield of the product are increased, and the crystal form of the product is good and easy to dry, thus the method is suitable for popularization and application in mass production.

Description

technical field [0001] The invention relates to the field of preparation of cefminox, in particular to a synthetic method of cefminox sodium. Background technique [0002] Cefminox sodium is a third-generation cephalosporin, which is a derivative of cephamycin. It is made of heptahydrate sodium salt by semi-synthetic method. It has good antibacterial effect on both Gram-negative and Gram-positive bacteria. There are mainly two types of synthesis methods: 1. Use 7β-aminocephalosporin derivatives as raw materials, protect the amino group with aldehyde or acyl halide, introduce trans-methoxy at the 7-position of the mother nucleus, remove the protecting group and then The acetylated product obtained by reacting with bromoacetyl bromide is further prepared into cefminox; 2. Using cephamycin derivatives (7β-amino-7α-methoxycephalosporin derivatives) as starting materials, in 7β- Amino and 3-positions are introduced into necessary side chains, protected by decarboxylation, and co...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/04
CPCC07D501/57C07D501/04
Inventor 许伟龙楼秋霞黄剑峰
Owner GUANGDONG LIGUO PHARMACY
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