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Method of synthesizing cefixime

A synthesis method and technology of cefixime, applied in the field of cefixime, can solve problems such as poor quality and low yield, and achieve the effects of improving yield, improving quality and yield, and reducing material loss

Inactive Publication Date: 2007-08-15
河源市制药工程技术研究开发中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the deficiencies in the above-mentioned prior art, and to provide a synthetic method for cefixime, which uses a cheaper inorganic salt to replace acetone, and combines the two-step reaction into a one-step reaction to realize the "one-pot cooking process" ", solved the problem of low yield and poor quality

Method used

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  • Method of synthesizing cefixime

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Add 300L of dichloromethane, 40kg of MICA-active ester into a clean reaction tank, add 25kg of AVNA, 100L of pure water, and 26L of triethylamine after dissolving, keep the temperature at 10°C, and react for 5.5 hours;

[0033] (2) Add 560L of ethyl acetate after the reaction, and extract with 300L of pure water at 5°C for 10 minutes;

[0034] (3) Stand still for 30 minutes to separate the liquid, mark the organic phase, recycle and pack into barrels; adjust the pH of the water phase to 7.0 with 36% acetic acid, add 400 L of ethyl acetate to extract for 20 minutes;

[0035] (4) Stand still for 30 minutes to separate the liquid, mark the organic phase, recycle and pack into barrels; add 400 L of ethyl acetate to the water phase to extract for 20 minutes, let stand for 30 minutes to separate the liquid, and recover the organic phase;

[0036] (5) Add 0.5kg of EDTA, 0.5kg of hydrosulfite, and 10kg of activated carbon to the water phase, and cool down and stir for 30 mi...

Embodiment 2

[0044] (1) Add 400L chloroform, 50kg MICA-active ester into a clean reaction tank, add 30kg AVNA, 136.4L pure water, 32.8L triethylamine after dissolving, keep the temperature at 15°C, and react for 4 hours;

[0045] (2) Add 680L of ethyl acetate after the reaction, and extract with 400L of pure water at 3°C ​​for 20 minutes;

[0046](3) Stand still for 60 minutes to separate liquids, mark the organic phase, recycle and pack into barrels; adjust the pH of the water phase to 6.2 with 36% acetic acid, add 450 L of ethyl acetate to extract for 30 minutes;

[0047] (4) Stand still for 60 minutes to separate the liquid, mark the organic phase, recycle and pack into barrels; add 450 L of ethyl acetate to the water phase to extract for 30 minutes, let stand for 60 minutes to separate the liquid, and recover the organic phase;

[0048] (5) Add 1kg of EDTA, 1kg of hydrosulfite, and 12kg of activated carbon to the water phase, and cool down and stir for 60 minutes to decolorize;

[004...

Embodiment 3

[0056] (1) Add 500L of dichloromethane, 45kg of MICA-active ester into a clean reaction tank, add 28kg of AVNA, 127L of pure water, and 30L of triethylamine after dissolving, keep the temperature at 13°C, and react for 3 hours;

[0057] (2) Add 630L of ethyl acetate after the reaction, and extract with 370L of pure water at 4°C for 15 minutes;

[0058] (3) Stand still for 50 minutes to separate the liquid, mark the organic phase, recycle and pack into barrels; adjust the pH of the water phase to 8.5 with 36% acetic acid, add 430 L of ethyl acetate to extract for 25 minutes;

[0059] (4) Stand still for 50 minutes to separate the liquid, mark the organic phase, recycle and pack into barrels; add 430 L of ethyl acetate to the water phase to extract for 25 minutes, stand still for 50 minutes to separate the liquid, and recover the organic phase;

[0060] (5) Add 0.8kg of EDTA, 0.8kg of hydrosulfite, and 11kg of activated carbon to the water phase, and cool down and stir for 45 mi...

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Abstract

The invention discloses a synthesizing method of cefuroxime, which is characterized by the following: crystallizing cefuroxime intermediate MECEF; synthesizing cefuroxime through water-phased extract of MECEF without dissolving MECEF; saving cost to improve receiving rate effectively; shortening manufacturing period.

Description

technical field [0001] The invention belongs to the technical field of cefixime in the chemical pharmaceutical industry, and in particular relates to a synthesis method of cefixime. Background technique [0002] Cefixime is a third-generation oral cephalosporin antibiotic, which has a broad-spectrum antibacterial effect on Gram-positive and Streptococcus), pneumococcus and Escherichia coli, Moraxella, Neisseria gonorrhoeae, Proteus mirabilis, and Cathaeria in Gram-negative bacteria showed stronger bactericidal effect than other oral cephalosporins. It has the characteristics of broad spectrum, high efficiency, enzyme resistance and low toxicity, and is an anti-infection oral drug widely used in clinical practice. [0003] The technical status of existing synthetic cefixime is as follows: [0004] (1) In a reaction tank with a thermometer and a nitrogen device that has replaced air, add MICA (cefixime side chain acid), accelerator DM (dibenzothiazole disulfide), triphenylph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22
Inventor 潘行远
Owner 河源市制药工程技术研究开发中心
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