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Preparation method of cefoperazone acid

A technology of cefoperazone acid and cefoperazone sodium, which is applied in the field of preparation of pharmaceutical intermediates, can solve problems such as difficult product quality assurance, complex synthesis reaction routes, and high raw material costs, and achieves no by-product formation, simple preparation process, and high preparation method simple effect

Active Publication Date: 2019-02-01
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis reaction route of this method is complex, and there are problems such as cumbersome operation, long reaction time, high cost of raw materials, darker product color, many by-products, and low yield in the industrial production process, and the product quality is difficult to be guaranteed.

Method used

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  • Preparation method of cefoperazone acid
  • Preparation method of cefoperazone acid
  • Preparation method of cefoperazone acid

Examples

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preparation example Construction

[0033] A preparation method of cefoperazone acid comprises the following steps: cefoperazone sodium is used as a raw material, a precipitating agent is added to a cefoperazone sodium solution to decolorize, and a dispersant is added to the decolorization solution for crystallization to obtain cefoperazone acid.

[0034] The quality index of cefoperazone sodium meets any one or a combination of total impurities > 3.0%, maximum single impurities > 2.0% or impurity A > 3.0%.

[0035] The preparation method comprises the following steps:

[0036] A. Add 2 to 5 times the quality of cefoperazone sodium in water to dissolve cefoperazone sodium, then add an organic solvent with 3 to 5 times the quality of cefoperazone sodium, stir and dissolve, and control the temperature during stirring to be 10 to 30°C to obtain a cefoperazone sodium solution;

[0037] The organic solvent is any one or a combination of acetone, acetonitrile or ethanol;

[0038] B. in the cefoperazone sodium solution,...

Embodiment 1

[0047] A preparation method of cefoperazone acid comprises the following steps: cefoperazone sodium is used as a raw material, a precipitating agent is added to a cefoperazone sodium solution to decolorize, and a dispersant is added to the decolorization solution for crystallization to obtain cefoperazone acid.

[0048] The preparation method comprises the following steps:

[0049] A. in 40g cefoperazone sodium (cefoperazone sodium total miscellaneous is 4.2%), add the water dissolving of 80mL, then add the acetone of 120mL, control stirring temperature is 10 ℃, stirring and dissolving is clear to dissolving, obtains cefoperazone sodium solution;

[0050] B. Add dropwise dipropylamine 8.62mL in the cefoperazone sodium solution, then add acetone 400mL, filter to obtain the precipitate;

[0051] C. The precipitate was adjusted to pH 5.0 with hydrochloric acid solution, and 0.4 g of activated carbon was added to decolorize for 1 hour. The filtrate was collected after decolorizing...

Embodiment 2～4

[0056] Embodiments 2 to 4 are identical to the production process steps in Example 1, and the difference is the selection of process parameters, as shown in Table 1 below, wherein "water addition" is the addition of milliliters of water to the mass grams of cefoperazone sodium How many times; "organic solvent addition" is how many times the milliliters of organic solvent is the mass grams of cefoperazone sodium; "the addition of dispersant" is how many times the milliliters of dispersant is the mass grams of cefoperazone sodium; "The amount of water added" is how many times the milliliters of purified water is the mass grams of cefoperazone sodium.

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Abstract

The invention discloses a preparation method of cefoperazone acid, and belongs to the field of preparation of medicinal intermediates. The preparation method comprises the following steps: a precipitating agent is added to a solution of cefoperazone sodium used as a raw material in order to decolorize the solution, a dispersant is added to the decolorized solution, and crystallization is carried out to obtain the cefoperazone acid. The method allows the cefoperazone sodium which does not meet quality standards to be fully recycled, the prepared cefoperazone acid has the advantages of high content, few impurities and good stability, and the preparation method has the advantages of simplicity, energy saving and environmental protection, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of a β-lactam antibiotic intermediate, and belongs to the field of preparation of pharmaceutical intermediates. Background technique [0002] Cefoperazone acid is white or off-white crystalline powder, chemical name 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]oct-2-ene-2-carboxylic acid. Cefoperazone acid is used to synthesize cefoperazone sodium. Cefoperazone sodium has certain stability to broad-spectrum β-lactamases produced by negative bacilli. It is used for the treatment of various infections caused by sensitive enzyme-producing bacteria, such as the respiratory system, genitourinary system, It is also effective in treating infections of the biliary tract, gastrointestinal tract, chest and abdomen, and skin and soft ...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/12C07D501/36
Inventor 贾全田洪年胡利敏张锁庆李庆伟石春利任峰刘树斌魏宝军贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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