Method for preparing cefotiam dihydrate dihydrochloride

A technology of cefotiam and dihydrochloride, which is applied in the field of preparation of cefotiam dihydrate dihydrochloride, can solve the problems of high product color grade, high impurity residue, poor reaction degree, etc., and achieve excellent color, The effect of less residual impurities and high content

Inactive Publication Date: 2008-01-02
HARBIN PHARMA GRP CO LTD GENERAL PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction degree of the above process is poor, the content of intermediates

Method used

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  • Method for preparing cefotiam dihydrate dihydrochloride
  • Method for preparing cefotiam dihydrate dihydrochloride
  • Method for preparing cefotiam dihydrate dihydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add acetonitrile, 31.54 g of 7-aminocephalosporanic acid, [(N,N)-dimethyl-amino-ethyl]-5-mercapto-tetrazolium at room temperature, and add trifluoride Boron-acetonitrile complex 185ml, time 5 hours when the temperature is raised to 20°C, add acetone, when the temperature is 18°C, add 37% hydrochloric acid and acetone dropwise, then add pre-cooled acetone, extract the material, wash with acetone, and obtain wet Taste. Add the wet product from the previous step to methanol and water, add carbon, stir, filter with suction, and wash with a mixture of methanol and water. Add triethylamine dropwise to the filtrate at a temperature of 15±5°C, then add methanol and water until pH = 3, stir for 1 hour at a temperature of 10°C, extract the material, wash with methanol and acetone successively, and drain to obtain [ 3-[[[(N,N)-Dimethyl-amino-ethyl-tetrazol-1-yl]thio]methyl]-8oxo-5-thia-1H-azabicyclo[4 , 2,0]oct-2-ene-2-carboxylic acid] hydrochloric acid solid 39.9g, high perform...

Embodiment 2

[0034] Add ether, 31.54g of 7-aminocephalosporanic acid, [(N,N)-dimethyl-amino-ethyl]-5-mercapto-tetrazolium, after complete dissolution, add boron trifluoride at 5°C -Ether complex 185ml, timed for 5 hours at a temperature of 20°C, sampling and measuring the 7-aminocephalosporanic acid content of 4.48%. Add acetone, drop hydrochloric acid and acetone when the temperature is 18°C, then add pre-cooled acetone. Stir for 30 minutes at a temperature of 10° C., extract the material, and wash with acetone to obtain a wet product. Add the wet product from the previous step to methanol and water, add carbon and stir for 30 minutes, filter with suction, and wash with a mixture of methanol and water. When the temperature of the filtrate is 15±5°C, add triethylamine, methanol and water dropwise, stir for 1 hour at a temperature of 10°C, extract the material, wash with methanol and acetone successively, and drain to obtain [3-[[[(N , N)-Dimethyl-amino-ethyl-tetrazol-1-yl]thio]methyl]-8 ...

Embodiment 3

[0036] At room temperature, add acetonitrile, dimethyl carbonate, 31.54 g of 7-aminocephalosporanic acid, [(N,N)-dimethyl-amino-ethyl]-5-mercapto-tetrazolium, and dissolve them completely at temperature Add 185ml of boron trifluoride-dimethyl carbonate complex at 5°C, control the temperature at 20°C and measure it online. When the content of 7-aminocephalosporanic acid is 4.84%, add acetone, and drop Add hydrochloric acid and acetone, then add pre-cooled acetone. Stir at 10°C for 30 minutes, extract the material, and wash with acetone to obtain a wet product. Add the wet product from the previous step to methanol and water, add carbon, stir for 30 minutes, filter with suction, and wash with a mixture of methanol and water. When the filtrate temperature is 15±5°C, add triethylamine, methanol 1, and water dropwise, stir at 10°C for 1 hour, take out the material, wash it with methanol and acetone successively, and dry it to obtain [3-[[[(N , N)-Dimethyl-amino-ethyl-tetrazol-1-y...

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Abstract

The invention discloses a synthesizing method of sterile raw material medicine of antibiotic medicine 7-[2-(2-amino thiazole-4-radical)acetylamino]-[3-[[[(N, N)-dimethyl-amino-ethyl-tetrazolium-1-radical] sulphur] methyl]-8 oxo-5-thio-1-azabicyclo [4, 2, 0] octa-2-olefin-2-carboxyl acid] hydrochloride dihydrate, which generates cephamtile with high content and good color and little impurity residual through adding sodium thiosulfate agent in the reflecting system to change the color of product cepham appearance.

Description

technical field [0001] The invention relates to a new preparation method of two antibacterial drugs cefotiam. Background technique [0002] Currently, the chemical name of cefotiam is: 7-[2-(2-aminothiazol-4-yl)acetamido]-[3-[[[(N,N)-dimethyl-amino-ethyl- Tetrazol-1-yl]thio]methyl]-8oxo-5-thia-1-azabicyclo[4,2,0]oct-2-ene-2-carboxylic acid]dihydrochloride dihydrate This product is the second-generation cephalosporin antibacterial drug for injection. The drug uses 7-aminocephalosporanic acid as the starting material, and introduces [(N , N)-dimethyl-amino-ethyl]-5-mercapto-tetrazolium heterocycle, and then the compound carries out nitrogen acylation reaction with formylamino-thiazolyl-4-acetic acid on the 7-position side chain . The reaction needs to use dichloromethane, methanol, N,N-dimethylacetyl chloride as a solvent, and boron trifluoride as a catalyst. The reaction degree of the above-mentioned technological process is poor, the intermediate content is low, the impu...

Claims

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Application Information

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IPC IPC(8): C07D501/36
Inventor 金乃岩朱彦民王彪张伟王宝宇张天娇赵飞
Owner HARBIN PHARMA GRP CO LTD GENERAL PHARMA FACTORY
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