Purification method of cefoperazone sodium

A technology of cefoperazone sodium and a purification method, which is applied in the field of purification of cefoperazone sodium, can solve the problems of complex synthetic route, cumbersome preparation process, and long process, and achieve the effect of high product content, low impurity content, and simple operation

Active Publication Date: 2021-01-29
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] "Preparation Method of Cefoperazone Sodium" (CN201310625115.5), "A Cefoperazone Sodium Compound and Its Preparation Utilizing the Principle of Fluid Mechanics" (CN106432273A) mainly introduce the method of using 7-ACA as the mother nucleus to synthesize cefoperazone sodium. long
[0006] A crystallization method of cefoperazone sodium (CN101863907B) in which cefoperazone acid is reacted with a salt-forming agent, and the cefoperazone sodium compound is obtained through secondary crystallization. At the same time, ultrasonic equipment is used, and the preparation process is cumbersome

Method used

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  • Purification method of cefoperazone sodium
  • Purification method of cefoperazone sodium
  • Purification method of cefoperazone sodium

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Take 80g of cefoperazone sodium and sulbactam sodium (the weight ratio of cefoperazone sodium and sulbactam sodium is 1:1, converted to 40g of cefoperazone sodium), add 160ml of purified water, control the temperature at 15°C, stir until dissolved, add 160ml of acetone, add 0.4g of activated carbon , decolorizing for 30min. Filter, wash with 5ml of purified water, combine the filtrate and washings, and set aside.

[0036] Add 800ml of acetone, 60ml of isopropanol, and 40ml of ethanol to the crystallizer; control the temperature of the crystallizer at 30-35°C, and add the above-mentioned filtrate and lotion while stirring at 400rpm / min. After the addition is completed, add sodium bicarbonate solution dropwise The pH of the solution is 6.6; after the adjustment, the temperature is controlled at 30-35°C and the crystal is grown for 180 minutes;

[0037] After the crystal growing, it took 60 minutes to cool down to 10°C, and then grow the crystal for 60 minutes. Filter, w...

Embodiment 2

[0039] Take 60g of cefoperazone sodium and sulbactam sodium (the weight ratio of cefoperazone sodium and sulbactam sodium is 2:1, converted to 40g of cefoperazone sodium), add 200ml of purified water, control the temperature at 10°C, stir until dissolved, add 200ml of acetone, add 0.4g of activated carbon , decolorizing for 30min. Filter, wash with 5ml of purified water, combine the filtrate and washings, and set aside.

[0040] Add 720ml of acetone, 20ml of isopropanol, and 20ml of ethanol to the crystallizer; control the temperature of the crystallizer at 30-35°C, and add the above-mentioned filtrate and lotion while stirring at 500rpm / min. After the addition is complete, add sodium bicarbonate solution dropwise The pH of the solution is 6.5; after the adjustment, the temperature is controlled at 30-35°C to grow the crystal for 210 minutes;

[0041] After the crystal growth is completed, it takes 90 minutes to cool down to 8°C, and then grow the crystal for 60 minutes. Fil...

Embodiment 3

[0043] Take 60kg of cefoperazone sodium and sulbactam sodium (the weight ratio of cefoperazone sodium and sulbactam sodium is 1:1, the conversion of cefoperazone sodium is 30kg), add 150L of purified water, control the temperature at 10°C, stir until dissolved, add 150L of acetone, add 0.3kg of activated carbon , decolorizing for 30min. Filter, wash with 5L of purified water, combine the filtrate and washings, and set aside.

[0044] Add 600L of acetone, 30L of isopropanol, and 30L of ethanol to the crystallizer; control the temperature of the crystallizer at 30-35°C, and add the above-mentioned filtrate and lotion while stirring at 450rpm / min. After the addition is complete, add sodium bicarbonate solution dropwise Liquid pH to 6.5; after adjustment, temperature control 30-35°C to grow crystal for 200min;

[0045] After the crystal growing, it took 180 minutes to cool down to 8°C, and then grow the crystal for 60 minutes. Filter, wash with 300L of 9:1 acetone-water mixture,...

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Abstract

The invention discloses a purification method of cefoperazone sodium, which comprises the steps of S1, adding a cefoperazone sodium and sulbactam sodium product into purified water, stirring until thesolution is clear, controlling the temperature, adding acetone into the reaction tank, and starting stirring until the cefoperazone sodium and sulbactam sodium are completely dissolved to obtain a dissolved solution; S2, adding activated carbon into the dissolved solution for decoloration, and filtering to obtain a destaining solution for later use; S3, adding acetone, isopropanol and ethanol into a crystallizer to obtain a mixed solution, and controlling the temperature of the crystallizer; S4, adding the destaining solution obtained in the step S2 into the crystallizer in a rapid stirring state, then dropwise adding a sodium bicarbonate solution to adjust the pH value of the feed liquid, and growing crystals; S5, after crystal growing is finished, cooling for crystal growing, filtering,and washing with an acetone-water mixed solution; and S6, conducting vacuum drying and discharging. The prepared cefoperazone sodium has the advantages of being stable in quality, low in impurity content and high in product content.

Description

technical field [0001] The invention relates to a method for purifying cefoperazone sodium, which belongs to the technical field of medicine. Background technique [0002] Cefoperazone sodium is a third-generation cephalosporin, which has certain stability to broad-spectrum β-lactamase produced by negative bacilli, and is used for the treatment of various infections caused by sensitive enzyme-producing bacteria, such as the respiratory system, genitourinary system, and biliary tract. , the treatment of gastrointestinal tract, thoracic and abdominal cavity, skin and soft tissue infections, and also has a good curative effect on brain infections caused by influenza bacillus and meningococcus. The chemical name of cefoperazone sodium is: (6R,7R)-3-[[(1-methyl-1H-tetrazol-5-yl)sulfur]methyl]-7-[(R)-2-(4-ethyl -2,3-dioxo-1-piperazinecarbonylamino)-2-p-hydroxyphenyl-acetylamino]-8-oxo-5-thia-1-azabicyclo[4.2.0]octane -2-ene-2-sodium carboxylate, the structural formula is as foll...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/12C07D501/36
CPCC07D501/12C07D501/36
Inventor 贾全田洪年张建丽任峰杨梦德魏宝军刘树斌贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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