Cefotiam hydrochloride crystal compound and preparation method thereof

A technology for cefotiam hydrochloride and crystalline compound, which is applied in the field of cefotiam hydrochloride crystalline compound and its preparation, can solve problems such as solvent residue and the like, and achieves low organic solvent residue, low moisture content and good stability Effect

Inactive 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

[0010] Aiming at the deficiencies in the prior art, the object of the present invention is to provide a cefotiam hydrochloride crystal form compound and its preparation method, which can solve the problem of solvent residue in common solvent crystallization and avoid a series of follow-up products caused by it. Quality problems, the method is safe and reliable, and the post-processing is simple and easy, which can effectively improve the quality of the product and provide a safety guarantee for the clinical application of cefotiam drugs

Method used

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  • Cefotiam hydrochloride crystal compound and preparation method thereof
  • Cefotiam hydrochloride crystal compound and preparation method thereof
  • Cefotiam hydrochloride crystal compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In liquid storage tank, add the mixed solvent of 500g 85% methanol / water, add cefotiam hydrochloride crude product 562g (1mol), control temperature 30 ℃, stir and make it dissolve, with the mixed solution in liquid storage tank Pump into the mixer, pump in CO with a high pressure liquid pump 2 Supercritical fluid to 20Mpa, stir at 30°C, and maintain the pressure and temperature for 15 minutes, turn off the high-pressure pump, place 6g of seed crystals in the precipitator, open the quick interface, let the liquid in the mixer completely enter the precipitator, close the quick Interface, adjust the pressure in the crystallization tank to 10Mpa, the temperature is 20°C, keep the temperature and pressure for 60 minutes, wait for the system to lower the temperature and pressure, and dry under reduced pressure at 50°C to obtain 534g of cefotiam hydrochloride crystals, with a yield of 95%.

Embodiment 2

[0034] In liquid storage tank, add the mixed solvent of 300g 85% methanol / water, add cefotiam hydrochloride crude product 562g (1mol), control temperature 30 ℃, stir and make it dissolve, with the mixed solution in the liquid storage tank Pump into the mixer, pump in CO with a high pressure liquid pump 2 Supercritical fluid to 20Mpa, stir at 30°C, and maintain the pressure and temperature for 15 minutes, turn off the high-pressure pump, place 6g of seed crystals in the precipitator, open the quick interface, let the liquid in the mixer completely enter the precipitator, close the quick Interface, adjust the pressure in the crystallization tank to 10Mpa, the temperature is 20°C, keep the temperature and pressure for 60 minutes, wait for the system to lower the temperature and pressure, and dry under reduced pressure at 50°C to obtain 502g of cefotiam hydrochloride crystals, with a yield of 94%.

Embodiment 3

[0036] In liquid storage tank, add the mixed solvent of 700g 85% methanol / water, add cefotiam hydrochloride crude product 562g (1mol), control temperature 30 ℃, stir and make it dissolve, with the mixed solution in the liquid storage tank Pump into the mixer, pump in CO with a high pressure liquid pump 2 Supercritical fluid to 20Mpa, stir at 30°C, and maintain the pressure and temperature for 15 minutes, turn off the high-pressure pump, place 6g of seed crystals in the precipitator, open the quick interface, let the liquid in the mixer completely enter the precipitator, close the quick Interface, adjust the pressure in the crystallization tank to 10Mpa, the temperature is 20°C, keep the temperature and pressure for 60 minutes, wait for the system to lower the temperature and pressure, and dry under reduced pressure at 50°C to obtain 421g of cefotiam hydrochloride crystals, with a yield of 75%.

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Abstract

The invention relates to the field of medicines and primarily relates to a cefotiam hydrochloride crystal compound and a preparation method thereof. The invention relates to a crystal form of cefotiam hydrochloride. The cefotiam hydrochloride crystal compound is characterized by being measured by a Cu-Kalpha ray. The primary characteristic peaks in an X-ray powder diffraction pattern are displayed when 2theta are 6.019 degrees, 11.542 degrees, 14.758 degrees, 16.699 degrees, 18.821 degrees, 19.100 degrees, 23.320 degrees, 23.521 degrees, 24.081 degrees, 26.101 degrees, 26.501 degrees, 30.160 degrees, 30.483 degrees, 31.700 degrees, 34.220 degrees, 34.502 degrees, 35.240 degrees and 38.020 degrees. The crystal form of cefotiam hydrochloride provided by the invention is high in sample purity, good in stability, low in water content, low in residue of an organic solvent, uniform in size distribution, good in flowability and suitable for package. The method provided by the invention is high in yield of production process and simple and easy to control.

Description

technical field [0001] The invention relates to the field of medicine, and mainly relates to a crystal compound 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
CPCC07B2200/13C07D501/12C07D501/36Y02P20/54
Inventor 叶天健陈鑫陈识峰蔡翔金彬书
Owner ZHEJIANG YONGNING PHARMA
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