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Method for crystallizing cefixime trihydrate

A technology for cefixime trihydrate and crystallization, which is applied in the field of cefixime preparation, can solve the problems of inconvenient industrial production and storage, low product quality, poor stability, etc. bad effect

Inactive Publication Date: 2012-06-27
ZHEJIANG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] No matter it is crystallized directly from water or crystallized by adding ethanol, the quality of the obtained product is not high (≤95%), especially the stability is generally poor, and the content is reduced by ≥5% after being placed at 40°C for one month, which brings problems to industrial production and storage. great inconvenience

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 500ml dry four-neck flask, add 300ml of purified water, add 20g (0.043mol) of dry cefixime methyl ester under stirring, after stirring evenly, cool to 0-2°C, add 170g of 3.7-4.0% NaOH solution, TCL After passing the test, control the temperature at 0-5°C, and add 14.6% hydrochloric acid solution to pH=5.1. After the adjustment, add 1.6g of activated carbon and stir for 30 minutes to decolorize. After decolorization, filter to obtain about 320ml of cefixime solution.

[0029] Add 32ml of ethanol and 8ml of acetone, raise the temperature to 25°C, and adjust the pH to 3.3 with 14.6% hydrochloric acid solution;

[0030] Raise the temperature of the solution by 5°C to 30°C, grow the crystal for 60 minutes, adjust the pH to 2.3 with 14.6% hydrochloric acid solution, and stir for 60 minutes;

[0031] Cool down to below 5°C and stir for 2h. filter. Vacuum drying below 35°C gave cefixime trihydrate 19.94g, yield 91.39%, content 99.51%, stability: 40°C for one month, con...

Embodiment 2

[0033] In a 500ml dry four-neck flask, add 300ml of purified water, add 20g (0.043mol) of dry cefixime methyl ester under stirring, after stirring evenly, cool to 0-2°C, add 170g of 3.7-4.0% NaOH solution, TCL After passing the test, control the temperature at 0-5°C, and add 14.6% hydrochloric acid solution to pH=5.2. After the adjustment, add 1.6g of activated carbon and stir for 30 minutes to decolorize. After decolorization, filter to obtain about 320ml of cefixime solution.

[0034] Add 8ml of ethanol and 60ml of acetonitrile, raise the temperature to 45°C, and adjust the pH to 3 with 14.6% hydrochloric acid solution;

[0035] Raise the temperature of the solution by 1°C to 46°C, grow the crystal for 180 minutes, adjust the pH to 2 with 14.6% hydrochloric acid solution, and stir for 90 minutes;

[0036] Cool down to below 5°C and stir for 2h. filter. Vacuum drying below 35°C yielded 18.58g of cefixime trihydrate with a yield of 85.16% and a content of 99.35%. Stability...

Embodiment 3

[0038] In a 500ml dry four-neck flask, add 300ml of purified water, add 20g (0.043mol) of dry cefixime methyl ester under stirring, after stirring evenly, cool to 0-2°C, add 170g of 3.7-4.0% NaOH solution, TCL After passing the test, control the temperature at 0-5°C, and add 14.6% hydrochloric acid solution to pH=5.0. After the adjustment, add 1.6g of activated carbon and stir for 30 minutes to decolorize. After decolorization, filter to obtain about 320ml of cefixime solution.

[0039] Add 60ml of ethanol, 8ml of ethyl acetate, the temperature is 25°C, adjust the pH to 3.3 with 14.6% hydrochloric acid solution;

[0040] Raise the temperature of the solution by 5°C to 30°C, grow the crystal for 60 minutes, adjust the pH to 2.3 with 14.6% hydrochloric acid solution, and stir for 60 minutes;

[0041] Cool down to below 5°C and stir for 2h. filter. Vacuum drying below 35°C yielded 18.90 g of cefixime trihydrate with a yield of 86.61% and a content of 99.54%. Stability: placed...

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PUM

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Abstract

The invention provides a method for crystallizing cefixime trihydrate. The cefixime trihydrate is obtained through hydrolyzing an aqueous solution of cefixime methyl ester by adding an alkali, adding at least one solvent, adjusting the pH value by an acid until the cefixime trihydrate is precipitated, heating, carrying out crystal growing for a certain time, and adjusting the pH value by the acid until a large amount of the cefixime trihydrate is precipitated. The method which allows at least one solvent to be added to water makes the impurity removal effect be very good and the cefixime trihydrate quality be high (equal to or more than 99.5%), and the obtained cefixime trihydrate has the advantages of granularity uniformity, good fluidity and very good stability, so the content is reduced by equal to or less than 0.2% after the cefixime trihydrate is disposed for 1 month at 40DEG C, thereby problems of bad quality and bad stability of the cefixime trihydrate in present domestic and foreign markets are solved, and the method is suitable for the industrialized production.

Description

technical field [0001] The invention relates to the technical field of preparation of cefixime, namely (6R,7R)-7-[[(Z)-2-(2-amino-4-thiazolyl)-2-[(carboxymethoxy)imino] Crystallization of acetyl]amino]-3-vinyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid trihydrate. Background technique [0002] Cefixime trihydrate is a new third-generation high-efficiency broad-spectrum oral cephalosporin antibiotic, which has a broad-spectrum antibacterial effect on Gram-positive bacteria and negative bacteria, and is used for the treatment of acute bacterial infectious diseases, upper and lower respiratory tract infections , pneumonia, acute bronchitis, acute attack of chronic bronchitis, urinary system infection, ear nose throat infection and other diseases. It has a long-lasting effective bactericidal concentration in the body, and its action strength is equivalent to that of the third-generation cephalosporin antibiotics for injection. [0003] [0004] The crystall...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/12C07D501/04
Inventor 邱家军吕秋波侯仲轲王宗利刘磊潘伯安肖秋霞
Owner ZHEJIANG GUOBANG PHARMA
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