Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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 the problems of solvent residue and the like, and achieves low organic solvent residue, good fluidity and low preparation cost. Effect

Inactive Publication Date: 2017-11-24
ZHEJIANG YONGNING PHARMA
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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
Comparison scheme
Effect test

Embodiment 1

[0024] In a 5000mL flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1200mL of methanol, add 150mL of concentrated hydrochloric acid and 600ml of ethyl acetate at 8°C, place the flask in an ultrasonic generator, and control the temperature at 23°C , turn on the ultrasonic seeding for 30 minutes, the ultrasonic frequency is 50KHz, and then stir for 30 minutes, then slowly add 600mL ethyl acetate to the flask, control the temperature at 8°C and crystallize for 2 hours, filter, wash the filter cake twice with 500mL ethyl acetate slurry , vacuum drying at 25° C. for 30 minutes, and then rising to 50° C. for 2 hours to obtain 555 g of cefotiam hydrochloride crystal form compound, with a yield of 98.8%.

Embodiment 2

[0026] In a 5000mL flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1200mL of DMF, add 150mL of concentrated hydrochloric acid and 600ml of ethyl acetate at 8°C, place the flask in an ultrasonic generator, and control the temperature at 23°C. Turn on the ultrasonic seeding for 30 minutes, the ultrasonic frequency is 50KHz, and then stir for 30 minutes, then slowly add 600mL ethyl acetate to the flask, control the temperature at 8°C and crystallize for 2 hours, filter, wash the filter cake twice with 500mL ethyl acetate slurry, Vacuum drying at 25°C for 30 minutes, and then vacuum drying at 50°C for 2 hours to obtain 168.6 g of cefotiam hydrochloride crystal form compound with a yield of 30%.

Embodiment 3

[0028] In a 5000mL flask, dissolve 562g (1mol) of crude cefotiam hydrochloride in 1200mL of methanol, add 75mL of concentrated sulfuric acid and 600ml of ethyl acetate at 8°C, place the flask in an ultrasonic generator, and control the temperature at 23°C , turn on the ultrasonic seeding for 30 minutes, the ultrasonic frequency is 50KHz, and then stir for 30 minutes, then slowly add 600mL ethyl acetate to the flask, control the temperature at 8°C and crystallize for 2 hours, filter, wash the filter cake twice with 500mL ethyl acetate slurry , vacuum drying at 25°C for 30min, and then rising to 50°C for vacuum drying for 2h to obtain 281g of cefotiam hydrochloride crystal form compound with a yield of 50%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the field of medicines, and mainly relates to a cefotiam hydrochloride crystal compound and a preparation method thereof. The cefotiam hydrochloride crystal compound is measured by using Cu-Ka rays, and main characteristic peaks are displayed at places that 2theta is 7.919 degrees, 11.361 degrees, 15.879 degrees, 18.341 degrees, 18.659 degrees, 19.159 degrees, 19.961, 21.922 degrees, 22.180 degrees, 22.682 degrees, 22.858 degrees, 23.883 degrees, 24.559 degrees, 26.197 degrees, 27.078 degrees, 27.339 degrees, 28.959 degrees, 29.380 degrees, 29.659 degrees, 31.061 degrees, 32.520 degrees, 33.021 and 36.379 degrees in an obtained X-ray powder diffraction pattern. The cefotiam hydrochloride crystal form provided by the invention 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, safe and reliable and applicable to large-scale production.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/36C07B2200/13C07D501/12
Inventor 叶天健陈鑫陈识峰蔡翔金彬书
Owner ZHEJIANG YONGNING PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com