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Novel crystal form of cefotiam hydrochloride and preparation method

A cefotiam hydrochloride and crystallization technology, applied in the field of medicine, can solve the problems of solvent residue and the like, and achieve the effects of low organic solvent residue, good fluidity and low preparation cost

Active Publication Date: 2017-11-24
ZHEJIANG YONGNING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the deficiencies in the prior art, the object of the present invention is to provide a cefotiam hydrochloride crystalline compound and a preparation method thereof, which can solve the problem of solvent residue in common solvent crystallization and avoid a series of follow-up product quality problems caused thereby. Problem, the method is safe and reliable, the post-processing is simple and easy, can effectively improve the quality of the product, and provides a safety guarantee for the clinical application of cefotiam drugs

Method used

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  • Novel crystal form of cefotiam hydrochloride and preparation method
  • Novel crystal form of cefotiam hydrochloride and preparation method
  • Novel crystal form of cefotiam hydrochloride and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In a flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1000mL of water, add 150mL of concentrated hydrochloric acid, 4000mL of ethanol, and 0.5mol of polyvinylpyrrolidone in sequence, heat to dissolve with microwave at 50°C, and slowly cool down to 25°C to stir and crystallize After 2 hours, filter, wash the filter cake twice with 200 mL of ethanol each, and dry it under vacuum at 45°C for 3 hours to obtain 545 g of cefotiam hydrochloride crystal form compound, with a yield of 97%.

Embodiment 2

[0026] In a flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1000mL of methanol, sequentially add 150mL of concentrated hydrochloric acid, 4000mL of ethanol, and 0.5mol of polyvinylpyrrolidone, heat to dissolve with microwave at 50°C, slowly cool down to 25°C and stir to analyze After crystallizing for 2 hours, filtering, washing the filter cake twice with 200 mL of ethanol each, and vacuum drying at 45° C. for 3 hours, 96 g of cefotiam hydrochloride crystal form compound was obtained, with a yield of 17%.

Embodiment 3

[0028] In a flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1000mL of water, add 150mL of concentrated sulfuric acid, 4000mL of ethanol, and 0.5mol of polyvinylpyrrolidone in sequence, heat to dissolve with microwave at 50°C, and slowly cool down to 25°C to stir and crystallize After 2 hours, filter, wash the filter cake twice with 200 mL of ethanol each, and dry it under vacuum at 45°C for 3 hours to obtain 39 g of cefotiam hydrochloride crystal form compound, with a yield of 7%.

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Abstract

The invention relates to the field of medicines, and mainly relates to a novel crystal form of cefotiam hydrochloride and a preparation method. The cefotiam hydrochloride compound is measured by using Cu-Ka rays, and main characteristic peaks are displayed at places that 2theta is 10.981 degrees, 14.959 degrees, 18.320 degrees, 19.141 degrees, 19.399 degrees, 23.121 degrees and 27.440 degrees in an obtained X-ray powder diffraction pattern. The cefotiam hydrochloride prepared by using the method is high in sample purity, good in stability, low in moisture, low in organic solvent residue, uniform in size distribution, good in flowability and applicable to sub-packaging. The preparation method provided by the invention is high in process yield, simple and convenient and easy to control, low in preparation cost and safe and reliable.

Description

technical field [0001] The invention relates to the field of medicine, and mainly relates to a new crystal form of cefotiam hydrochloride and a preparation method thereof. Background technique [0002] Cefotiam, also known as (6R-trans)-7-[[(2-amino-4-thiazolyl)acetyl]amino]-3-[[[1-[(2-(Dimethylamino)ethyl Base]-1H-tetrazol-5-yl]thiomethyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disalt salt. Its structural formula is: [0003] [0004] Cefotiam was first developed by Takeda Pharmaceutical Co., Ltd. in Japan. The product is dihydrochloride, and a certain amount of anhydrous sodium carbonate is added. Its dihydrochloride is commonly used, which is white or slightly yellow powder; it has a slightly specific odor; it dissolves effervescently with water to form a near-neutral transparent solution, which is slightly soluble in ethanol and insoluble in acetone and chloroform. [0005] This product is a second-generation cephalosporin antibiotic. The effe...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
CPCC07B2200/13C07D501/12C07D501/36
Inventor 叶天健陈鑫陈识峰蔡翔金彬书
Owner ZHEJIANG YONGNING PHARMA
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