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New method for purifying cefotiam hydrochloride

A kind of cefotiam hydrochloride, the technology of preparation method, applied in the field of medicine, can solve the problem of low purity of cefotiam hydrochloride and the like

Inactive Publication Date: 2011-09-21
HAINAN LINGKANG PHARMA 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 low purity of cefotiam hydrochloride prepared by the prior art, the invention provides a method for refining cefotiam hydrochloride compound

Method used

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  • New method for purifying cefotiam hydrochloride
  • New method for purifying cefotiam hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Take 10 g of crude cefotiam hydrochloride prepared according to CN101633666B, the content of cefotiam as measured by high performance liquid chromatography is 75%, and the content of polymer as determined by gel chromatography system is 3%. The cefotiam hydrochloride crude product was dissolved in 200ml of water, treated with 20ml of 1M sodium bisulfate aqueous solution, the treatment temperature was 30°C, and the treatment time was 2 hours, then cooled to room temperature, a precipitate was precipitated, and the aqueous filtrate was obtained after filtration .

[0064] Ethyl acetate was added to the above aqueous solution to extract twice, each time the volume of the solvent used accounted for 40% of the volume of the aqueous solution, after being fully stirred, left to stand, and then the organic phase was separated to obtain an aqueous phase containing cefotiam hydrochloride.

[0065] The obtained cefotiam hydrochloride aqueous solution is raised to 45 DEG C and conc...

Embodiment 2

[0070] Get 10g cefotiam hydrochloride bulk drug (produced by Jiangsu Jiuzhitang Biological Products Co., Ltd., the year of production in August, 2010), the content of cefotiam recorded by high performance liquid chromatography is 79.5%, and the polymer content measured by gel chromatography system is 0.5%. Dissolve the crude product of cefotiam hydrochloride in 150ml of water, and treat it with 15ml of 2M potassium bisulfate aqueous solution. The treatment temperature is 40°C, and the treatment time is 1 hour. filtrate.

[0071] Cyclohexane was added to the aqueous solution for extraction three times, each time the volume of the solvent used accounted for 30% of the volume of the aqueous solution. After fully stirring, the mixture was allowed to stand, and then the organic phase was separated to obtain an aqueous phase containing cefotiam hydrochloride.

[0072] The obtained cefotiam hydrochloride aqueous solution is raised to 48 ℃ and concentrated, and concentrated to a solu...

Embodiment 3

[0075] Get the longer cefotiam hydrochloride raw material drug (Shanghai New Pioneer Pharmaceutical Co., Ltd. production, batch number 20080912) of 10g production date, the content of cefotiam recorded by high-performance liquid chromatography is 77.5%, and the gel chromatography system assay polymer The content is 2.5%. The cefotiam hydrochloride crude product was dissolved in 250ml of water, and treated with 30ml of 1M potassium bisulfate aqueous solution, the treatment temperature was 35°C, and the treatment time was 3 hours, then the temperature was cooled to room temperature, a precipitate was precipitated, and the aqueous filtrate was obtained after filtration .

[0076] Add cyclohexane and ethyl acetate 1:1 mixed solvent to the above aqueous solution and extract 3 times, the volume of the solvent used each time accounts for 25% of the volume of the aqueous solution, after fully stirring, let it stand, and then separate the organic phase to obtain An aqueous phase conta...

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Abstract

The invention relates to a method for purifying cefotiam hydrochloride, which comprises the following steps of: 1) dissolving a raw material of cefotiam hydrochloride in water, treating by using an acid salt substance, reducing temperature, and filtering off a precipitate separated out so as to obtain water-containing filtrate; 2) adding a solvent immiscible with water into the aqueous solution for extraction, separating to remove an organic phase containing impurities, and obtaining aqueous solution containing the cefotiam hydrochloride; and 3) adding a poor solvent of the cefotiam hydrochloride into the aqueous solution, controlling temperature for recrystallization, centrifugally washing crystals separated out, and drying to obtain the purified cefotiam hydrochloride. The refined cefotiam hydrochloride purified by the method has the cefotiam hydrochloride content of not less than 86 percent and the polymer impurity content of less than 3 percent; and injection prepared from the purified cefotiam hydrochloride has extremely low insoluble particle content.

Description

technical field [0001] The invention relates to a new preparation method for purifying cefotiam hydrochloride, which belongs to the technical field of medicine. Background technique [0002] Cefotiam hydrochloride is a semi-synthetic second-generation cephalosporin with the chemical name (6R,7R)-7-[[(2-amino-4-thiazolyl)acetyl]amino]-3-[ [1-[2-(Dimethylamino)ethyl]-1H-tetrazol-5-yl]thiomethyl]-8-oxo-5-thia-1-azabicyclo[4,2, 0] Oct-2-ene-2-carboxylic acid dihydrochloride, with many aliases in Chinese, such as cefotiam dihydrogen chloride, cefotiam hydrochloride, cefotazone, pansborin, and vansperine , Thietamazole cephalosporin, cefotazol, cefotiam, cefotiam dihydrochloride, pansperm, etc. Molecular formula is C 18 h 25 C 12 N 9 o 4 S 3 , the molecular weight is 598.55, CAS No.: 66309-69-1, and the boiling point at 760mmHg is 940°C. Flash point: 522.3°C. Calculated as anhydrous matter, the content of cefotiam should not be less than 79.0%. The structural formula is...

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 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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