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Novel method for preparing cefmenoxime hydrochloride compound

A technology of cefmenoxime hydrochloride and its compound, which is applied in the field of new preparation methods for purifying cefmenoxime hydrochloride, and can solve the problems of low purity of cefmenoxime hydrochloride

Active Publication Date: 2012-01-25
LIONCO PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to overcome the defects of the above-mentioned prior art, especially the defect of low purity of cefmenoxime hydrochloride prepared by the prior art, the invention provides a method for refining cefmenoxime hydrochloride compound

Method used

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  • Novel method for preparing cefmenoxime hydrochloride compound
  • Novel method for preparing cefmenoxime hydrochloride compound
  • Novel method for preparing cefmenoxime hydrochloride compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Take 100 g of crude cefmenoxime hydrochloride prepared according to CN101555251A, the content of cefmenoxime hydrochloride as measured by high performance liquid chromatography is 89%, and the content of polymer as determined by gel chromatography system is 4%. Add ethanol to the raw material cefmenoxime hydrochloride, control the temperature not to exceed 28°C, stir vigorously, and then filter, wash the filter cake with ethanol at a temperature not exceeding 20°C, and air dry.

[0061] The filter cake is put into 20% ammonia water, and the treatment time is 2 hours, until the aqueous solution reaches weak alkalinity, preferably with a pH value not exceeding 8.5. Stirring is carried out during the treatment, and the separated precipitate is filtered off. Then the aqueous solution was heated to 40°C to remove the remaining ammonia gas components in the aqueous solution.

[0062] Slowly add hydrochloric acid with a concentration of 2 mol / L to the obtained ammonia solutio...

Embodiment 2

[0071] Get 100g cefmenoxime hydrochloride bulk drug (produced by Zhejiang Jianfeng Pharmaceutical Co., Ltd., batch number 20110203), the purity of cefmenoxime recorded by high performance liquid chromatography is 91%, and the polymer impurity content measured by gel chromatography is 1.5%. Add ethyl acetate to the raw material cefmenoxime hydrochloride, control the temperature not to exceed 25°C, stir vigorously, and then filter, wash the filter cake with ethyl acetate at a temperature not exceeding 16°C, and dry in vacuum.

[0072] The filter cake is put into 23% ammonia water, and the treatment time is 3 hours, until the aqueous solution reaches weak alkalinity, preferably the pH value is not more than 9. Stirring is carried out during the treatment, and the separated precipitate is filtered off. Then the aqueous solution was heated to 45°C to remove the remaining ammonia gas components in the aqueous solution.

[0073] Slowly add hydrochloric acid with a concentration of 3...

Embodiment 3

[0076] Get 100g of cefmenoxime hydrochloride crude drug (produced by Zhejiang Jianfeng Pharmaceutical Co., Ltd., batch number 20080701) with a longer production date, the purity of cefmenoxime recorded by high performance liquid chromatography is 85%, and the determination of macromolecular impurities by gel chromatography Content 9%. Add ethyl acetate to the raw material cefmenoxime hydrochloride, control the temperature not exceeding 25°C, stir vigorously, and then filter, wash the filter cake with ethyl acetate at a temperature not exceeding 15°C, and dry it in vacuum.

[0077] Put the filter cake into ammonia water with a concentration of 20%, and the treatment time is 4 hours, until the aqueous solution reaches weak alkalinity, preferably the pH value is not more than 8. Stirring is carried out during the treatment, and the separated precipitate is filtered off. Then the aqueous solution was heated to 50°C to remove the remaining ammonia gas components in the aqueous sol...

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Abstract

The invention relates to a novel method for preparing a cefmenoxime hydrochloride compound. The method comprises the following steps of: 1) adding a cefmenoxime hydrochloride-insoluble solvent into a raw material, namely cefmenoxime hydrochloride, controlling the temperature to be not more than 30 DEG C, violently stirring, filtering, washing a filter cake by using the cefmenoxime hydrochloride-insoluble solvent at the temperature of not more than 20 DEG C, and performing vacuum drying or air-drying; 2) putting the filter cake into ammonia water, mildly stirring, controlling the pH value to be not more than 9 so as to obtain an ammonia water solution of cefmenoxime acid, and filtering a precipitate; 3) slowly adding hydrochloric acid at the concentration of between 0.5 and 4mol / L into the ammonia water solution of the cefmenoxime acid, controlling the temperature to be 30 to 60 DEG C, finally controlling the pH value to be 0.5 to 3.0, keeping for 30 minutes to 5 hours so as to slowly precipitate crystals, gradually reducing the temperature to the lowest 10 DEG C, standing, crystallizing, performing suction filtration, and performing vacuum drying to obtain a refined product of the cefmenoxime hydrochloride; and 4) optionally, returning crystallization mother liquor obtained after the crystals are precipitated to step 3). By the method, the purity of the cefmenoxime hydrochloride is greatly improved, the content of related substances is remarkably reduced, the quality of preparation products is improved, and the toxic or side effect is reduced.

Description

technical field [0001] The invention relates to a new preparation method for purifying cefmenoxime hydrochloride, which belongs to the technical field of medicine. Background technique [0002] The chemical name of cefmenoxime hydrochloride is (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-methoxyiminoacetamido]-3-[ [(1-Methyl-1H-tetrazol-5-yl)-thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2 -Formic acid hydrochloride (2:1), has many aliases in Chinese, such as Besterke; Cefaxime cephalosporin; Cefmenoxime; Cephaloxime hydrochloride and Cefotaxime. The molecular formula is (C 16 h 17 N 9 o 5 S 3 ) 2 HCl, the molecular weight is 1059.58, and the structural formula is: [0003] [0004] Cephalosporin antibiotics belong to β-lactam antibiotics, which are the most rapidly developed and most new types of antibiotics at home and abroad in recent years, and are highly effective and low-toxic antibiotics. Cefmenoxime hydrochloride is a third-generation semi-synthetic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/00C07D501/57
Inventor 陶灵刚
Owner LIONCO PHARM GRP CO LTD
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