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A kind of preparation method of cefamandole sodium

A technology of cefamandole sodium and aminocephalosporanic acid, which is applied in the field of medicine, can solve the problems of high production cost, waste of energy consumption, complicated preparation process and the like, and achieve the effects of reducing production cost, shortening technological process and simple preparation method.

Active Publication Date: 2018-05-15
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent application, steps such as concentration and recrystallization are required when obtaining formyl cefamandole acid, and recrystallization treatment is required when obtaining cefamandole sodium, which makes the preparation process more cumbersome and consumes more energy. , higher production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Pump 184L of acetonitrile into the 500L reactor, add 28.75kg of 7-aminocephalosporanic acid and 13.5kg of mercaptotetrazolium into the reactor, rinse the wall of the kettle with 5L of acetonitrile, lower the system temperature to 5°C, and then pump Inject 132.25L of boron trifluoride acetonitrile as a catalyst, flush the pipeline with 5L of acetonitrile, raise the temperature of the system to 28-32°C and stir for 3 hours, then cool the system to 0-5°C, input the solution in the system through a feeding pump or vacuum pump Put it into another 1000L reactor with 210L of deionized water at 5°C, stir for 30 minutes until cloudy, add 60L of 10% ammonia water dropwise at 0-5°C to make the pH of the system 2.4-2.6, and stir for 60 minutes , centrifuged and filtered to obtain crystals, the crystals were washed three times with 80L of acetonitrile and water with a volume ratio of 7:3, three times with 80L water, and three times with 80L acetone. ℃, dried for 8 hours to obtai...

Embodiment 2

[0036] (1) Pump 184L of acetonitrile into the 500L reactor, add 28.75kg of 7-aminocephalosporanic acid and 13.5kg of mercaptotetrazolium into the reactor, rinse the wall of the kettle with 5L of acetonitrile, lower the system temperature to 5°C, and then pump Inject 132.25L of boron trifluoride acetonitrile as a catalyst, flush the pipeline with 5L of acetonitrile, raise the temperature of the system to 28-32°C and stir for 3 hours, then cool the system to 0-5°C, input the solution in the system through a feeding pump or vacuum pump Put it into another 1000L reactor with 210L of deionized water at 5°C, stir for 30 minutes until cloudy, add 60L of 10% ammonia water dropwise at 0-5°C to make the pH of the system 2.4-2.6, and stir for 60 minutes , centrifuged and filtered to obtain crystals, the crystals were washed three times with 80L of acetonitrile and water with a volume ratio of 7:3, three times with 80L water, and three times with 80L acetone. ℃, dried for 8 hours to obtai...

Embodiment 3

[0039] (1) Pump 184L of acetonitrile into the 500L reactor, add 28.75kg of 7-aminocephalosporanic acid and 13.5kg of mercaptotetrazolium into the reactor, rinse the wall of the kettle with 5L of acetonitrile, lower the system temperature to 5°C, and then pump Inject 132.25L of boron trifluoride acetonitrile as a catalyst, flush the pipeline with 5L of acetonitrile, raise the temperature of the system to 28-32°C and stir for 3 hours, then cool the system to 0-5°C, input the solution in the system through a feeding pump or vacuum pump Put it into another 1000L reactor with 210L of deionized water at 5°C, stir for 30 minutes until cloudy, add 60L of 10% ammonia water dropwise at 0-5°C to make the pH of the system 2.4-2.6, and stir for 60 minutes , centrifuged and filtered to obtain crystals, the crystals were washed three times with 80L of acetonitrile and water with a volume ratio of 7:3, three times with 80L water, and three times with 80L acetone. ℃, dried for 8 hours to obtai...

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PUM

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Abstract

The invention relates to a preparation method for sodium cefamandole. The preparation method comprises mixing 7-aminocephalosporanic acid, 5-mercapto-1-methyltetrazole and a catalyst boron trifluoride acetonitrile complex, heating and stirring for reacting, cooling and processing to obtain a compound 1; performing heating refluxing reaction on the compound 1 and a silanization agent until the solution is clear, adding N,N-dimethylaniline under protection of inert gas, and dropwise adding (D)-(-)-O-formylmandeloyl chloride for chloroformylation reaction, after the reaction is finished, adding water for hydrolysis, adjusting the pH value to 5.0-7.5 by using a sodium bicarbonate or sodium carbonate solution, separating out the organic layer, adding ethyl acetate into the water layer, and adjusting the pH value to 0.5-1.5, so as to obtain a cephamandole solution, performing decoloring and dewatering, then adding an organic solution of sodium isooctanoate or sodium acetate, and crystallizing to obtain sodium cefamandole. The preparation technology is simple and easy to realize, the obtained product is shallow in color grade, impurity is less, yield is high, and the solvent is easy to recover and reuse, and thus production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of cefamandole sodium. Background technique [0002] Cefamandole sodium, also known as ceftriaxone, is a second-generation cephalosporin that is positive for Gram-negative bacteria, meningococcus, Clostridium anaerobes, Neisseria gonorrhoeae, Klebsiella pneumoniae, Escherichia coli, and indole Proteus and influenza bacilli have strong effects, especially for Haemophilus cefamandole sodium is the most effective. Clinically, cefamandole sodium is mainly used for various infections caused by sensitive bacteria, such as respiratory tract infection, pyelonephritis, biliary tract infection, peritonitis, urinary tract infection, sepsis and skin soft tissue, joint, bone and other infections. [0003] The preparation technology of cefamandole sodium mainly comprises three kinds of synthetic routes at present: the first is to synthesize cefamandole sodium...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06C07D501/12
CPCC07D501/06C07D501/12C07D501/36
Inventor 周自金罗新祖钱志勇汪飞强刘要武张波钟建西张群芳
Owner 苏州盛达药业有限公司
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