Preparation method of high-purity cefoperazone sodium micro powder

A technology of cefoperazone sodium micropowder and cefoperazone sodium, applied in the field of medicine, can solve problems such as solvent residues that cannot be effectively solved, and achieve the effects of high product yield and purity, few by-products, and avoiding oxidation

Active Publication Date: 2019-05-24
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Patent CN106432273A discloses a method for preparing cefoperazone sodium compound and its preparation using the principle of hydrodynamics, using dropwise crystallization of acetone, which also has the problem of being unable to effectively solve the problem of solvent residue in the product

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  • Preparation method of high-purity cefoperazone sodium micro powder
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  • Preparation method of high-purity cefoperazone sodium micro powder

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preparation example Construction

[0029] A preparation method of high-purity cefoperazone sodium micropowder, comprising: using cefoperazone acid as a raw material, first preparing a cefoperazone sodium solution, and then performing decolorization treatment, adding the decolorized cefoperazone sodium solution into a reaction kettle fed with a supercritical fluid, and crystallizing to obtain Cefoperazone Sodium Micropowder.

[0030] Concrete preparation method comprises the following steps:

[0031] A. Add cefoperazone acid to an organic solvent, add an alkaline sodium-containing reagent to adjust the pH to 6.5-7.0, and obtain a cefoperazone sodium solution; wherein the organic solvent is any one of acetone, ethanol, and isopropanol, and the alkaline sodium-containing The reagent is any aqueous solution of sodium bicarbonate, sodium carbonate or sodium hydroxide.

[0032] B. add decolorizing agent in the cefoperazone sodium solution and carry out decolouring, obtain filtrate and filter cake after filtering, wa...

Embodiment 1

[0039] A preparation method of high-purity cefoperazone sodium micropowder, comprising: using cefoperazone acid as a raw material, first preparing a cefoperazone sodium solution, and then performing decolorization treatment, adding the decolorized cefoperazone sodium solution into a reaction kettle fed with a supercritical fluid, and crystallizing to obtain Cefoperazone Sodium Micropowder.

[0040] Concrete preparation method comprises the following steps:

[0041] A. 10g cefoperazone acid is added in 100L acetone, and aqueous sodium bicarbonate solution is adjusted pH to 6.5, obtains cefoperazone sodium solution;

[0042] B. Decolorize the gac that accounts for 10% of the quality of the cefoperazone sodium solution in the cefoperazone sodium solution. The decolorization time is 30 to 60 minutes. After filtering, the filtrate and filter cake are obtained, and then the filter cake is washed, and the eluate and the filtrate are combined to obtain the decolorized cefoperazone sod...

Embodiment 2

[0048] A preparation method of high-purity cefoperazone sodium micropowder, comprising: using cefoperazone acid as a raw material, first preparing a cefoperazone sodium solution, and then performing decolorization treatment, adding the decolorized cefoperazone sodium solution into a reaction kettle fed with a supercritical fluid, and crystallizing to obtain Cefoperazone Sodium Micropowder.

[0049] Concrete preparation method comprises the following steps:

[0050] A. 30g cefoperazone acid is added in 100L ethanol, and sodium carbonate aqueous solution is adjusted pH to 7.0, obtains cefoperazone sodium solution;

[0051] B. decolorize the gac that accounts for 1% of the quality of the cefoperazone sodium solution in the cefoperazone sodium solution, the decolorization time is 30~60min, obtain the filtrate and filter cake after filtration, then wash the filter cake, obtain the decolorized cefoperazone sodium solution after the eluate and the filtrate are combined , the concent...

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Abstract

The invention discloses a preparation method of high-purity cefoperazone sodium micro powder, and belongs to the technical field of medicines. Cefoperazone acid is taken as a raw material, a cefoperazone sodium solution is prepared first, decolorizing treatment is then conducted, the decolorized cefoperazone sodium solution is added to a reaction kettle to which a super-critical fluid is added, and the cefoperazone sodium micro powder is obtained through crystallization. The preparation method has the advantages that the process is stable, the micro powder is green and environmentally friendly, the oxidation of a product can be avoided, the prepared cefoperazone sodium micro powder has the advantages of high purity and less impurity, the particle fluidity of the product is good, and the granularity is controllable.

Description

technical field [0001] The invention relates to cephalosporins, in particular to cefoperazone sodium, and belongs to the technical field of medicine. Background technique [0002] 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-carboxylic acid sodium salt, white to light yellow powder or crystalline powder, easily soluble in water, slightly soluble in methanol, very slightly soluble in ethanol, insoluble in acetone or ethyl acetate; used for sensitive products The treatment of various infections caused by enzyme bacteria, such as the treatment of respiratory system, genitourinary system, biliary tract, gastrointestinal tract, chest and abdominal cavity, skin and soft tissue infections, and the intracerebral infection caused by influenza bacillus and meningococcus. curative effect. Its struc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCY02P20/54
Inventor 魏宝军贾全任峰田洪年刘树斌贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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