Cefditoren pivoxil purifying method

A technology of cefditoren pivoxil and a refining method, which is applied in the field of medicine and chemical industry, can solve the problems of low product purity and cumbersome industrial production, and achieve the effect of simple operation and easy industrial production operation

Inactive Publication Date: 2016-12-21
JINAN KANGHE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] For solving the problem that cefditoren pivoxil gained product purity is lower, industrialized production is loaded down with trivial d...

Method used

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  • Cefditoren pivoxil purifying method

Examples

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Effect test

Embodiment 1

[0031] Embodiment 1: the preparation of cefditoren pivoxil refined product

[0032] (1) Add 70mL ethyl acetate and 14g crude cefditoren pivoxil to a 250mL reaction flask, stir and cool to 0°C, add 98mL 5% hydrochloric acid solution, stir for 10min, and separate the liquids; The solution was extracted once, the water layers were combined, the water layer was washed with 70mL ethyl acetate, and the layers were separated, and the obtained water layer was cefditoren pivoxil salt solution; 70mL dichloromethane was added to the water layer, stirred and cooled to 0°C, Add 8% sodium bicarbonate solution, adjust the pH to 5.0 within 1 h, separate the layers, wash the organic layer twice with saturated aqueous sodium chloride solution, 100 mL each time, add 4.2 g of anhydrous magnesium sulfate and 1.4 g of drug Use activated carbon, dry and decolorize at 0°C for 0.5h, filter, wash the filter cake with 10mL of dichloromethane, combine the filtrate and washing liquid, the filtrate is an o...

Embodiment 2

[0035] Embodiment 2: the preparation of cefditoren pivoxil refined product

[0036](1) Add 100mL n-butyl acetate and 20g crude cefditoren pivoxil to a 500mL reaction flask, stir and cool down to 25°C, add 120mL 5% sulfuric acid solution, stir for 10min, and separate the liquids; Extract with sulfuric acid solution once, combine the water layers, wash the water layer with 100mL n-butyl acetate, separate the layers, the obtained water layer is cefditoren pivoxil salt solution; add 100mL1,2-dichloroethane to the water layer, stir Cool down to 5°C, add 4% sodium hydroxide solution dropwise, adjust the pH to 8.0 within 1 h, separate the layers, wash the organic layer twice with saturated aqueous sodium chloride solution, 150 mL each time, add 5.0 g of anhydrous Magnesium sulfate and 2.0g of pharmaceutical activated carbon, dry and decolorize at 10°C for 0.5h, filter, wash the filter cake with 15mL of 1,2-dichloroethane, combine the filtrate and wash, the filtrate is the organic sol...

Embodiment 3

[0039] Embodiment 3: the preparation of cefditoren pivoxil refined product

[0040] (1) Add 70mL of dichloromethane and 14g of crude cefditoren pivoxil to a 250mL reaction flask, stir and cool down to -10°C, add 98mL of 5% nitric acid solution, stir for 10min, and separate the liquids; Nitric acid solution was extracted once, and the aqueous layers were combined; the aqueous layer was washed with 70 mL of dichloromethane, and separated, and the obtained aqueous layer was cefditoren pivoxil salt solution; 70 mL of ethyl acetate was added to the aqueous layer, stirred and cooled to 5 ° C, Add 8% sodium carbonate solution dropwise, adjust the pH to 7.0 within 1 h, separate the liquids, wash the organic layer twice with saturated aqueous sodium chloride solution, 100 mL each time, add 4.2 g of anhydrous magnesium sulfate and 1.4 g of medicine to the organic layer. Use activated carbon, dry and decolorize at 0°C for 0.5h, filter, wash the filter cake with 10mL ethyl acetate, combin...

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Abstract

The invention relates to a cefditoren pivoxil purifying method. The method concretely comprises the following steps: dissolving crude cefditoren pivoxil with low purity in an organic solvent, adding an acid to form a salt, washing the salt, carrying out liquid separation, adding an organic solvent, adjusting the pH value of the obtained solution to 4.0-8.0 by using an alkali, adding the above obtained organic layer to a non-polar solvent in a dropwise manner to obtain an amorphous solid, and crystallizing the amorphous solid by using an organic solvent to obtain purified cefditoren pivoxil with a crystal form. The purity of the final product is 99.0-99.7%, the content of E-isomer is smaller than 0.1%. The method has the advantages of simplicity in operation, mild reaction conditions, obvious improvement of the purity of the product, and facilitation of industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for refining cefditoren pivoxil. technical background [0002] Cefditoren pivoxil, the Chinese chemical name is 2,2-dimethylpropionyloxymethyl(6R,7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2- Methoxyiminoacetamido]-3-[(Z)-2-(4-methyl-1,3-thiazol-5-yl)ethenyl]-8-oxo-5-thia-1- Azabicyclo[4.2.0]oct-2-ene-2-carboxylate, English name: Cefditren Pivoxil, the raw material is light yellow-white to yellow crystalline powder, dissolved in dilute hydrochloric acid, slightly soluble in methanol, slightly Soluble in acetonitrile and ethanol (95%), very slightly soluble in ether, almost insoluble in water; molecular weight: 620.72. [0003] Cefditoren pivoxil is the third-generation cephalosporin antibacterial drug, developed by Japan Meiji Seika Co., Ltd., and listed in Japan under the trade name Meiact in 1994. my country approved the listing of tablets ...

Claims

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Application Information

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IPC IPC(8): C07D501/24C07D501/12
CPCC07D501/12C07D501/24
Inventor 张颖郑钧飞吴占营陈启绪
Owner JINAN KANGHE MEDICAL TECH
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