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Preparation method of cefozopran hydrochloride intermediate

A technology of cefazolam hydrochloride and cefazolam, which is applied in the field of preparation of cefazolam hydrochloride intermediates, can solve problems such as poor stability, decreased purity, easy hydrolysis, etc., and achieves the advantages of shortening reaction time, reducing by-products and low cost. Effect

Pending Publication Date: 2022-04-12
HAINAN HAILING CHEMIPHARMA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using 7-aminocephalosporanic acid (7-ACA) as raw material to prepare intermediate 7-ACP, due to physical properties such as easy hydrolysis and poor stability of the raw material, it is easy to produce by-products in the preparation process, resulting in a decrease in purity

Method used

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  • Preparation method of cefozopran hydrochloride intermediate
  • Preparation method of cefozopran hydrochloride intermediate
  • Preparation method of cefozopran hydrochloride intermediate

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Experimental program
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Embodiment 1

[0027] The preparation method of embodiment 1 cefozopran hydrochloride intermediate

[0028] (1) Using 7-ACA as the starting material, mix and react 7-ACA, hexamethyldisilazane and iodotrimethylsilane at a mass ratio of 1:1.7:0.6 for 2.5 hours at a reaction temperature of 23°C to prepare Compound 1 was obtained.

[0029] (2) Compound 1 and imidazo[1,2-b]pyridazine with a mass ratio of 1:2 are mixed with a solvent, the volume ratio of the compound 1 and the solvent is 1:15, and the volume ratio of the solvent is 1 : 2 mixed solution of dimethylformamide and dichloromethane, reacted for 3.5h, and the reaction temperature was 23°C to obtain compound 2.

[0030] (3) preparation mass concentration is 6% phosphoric acid acetonitrile solution, compound 2 is added in phosphoric acid acetonitrile solution and reacts 50min, and reaction temperature is 23 ℃, and described compound 2 and phosphoric acid acetonitrile solution volume ratio are 1:5, make ceftizole Blue intermediate crude. ...

Embodiment 2

[0032] The preparation method of embodiment 2 cefozopran hydrochloride intermediate

[0033] (1) Using 7-ACA as the starting material, mix and react 7-ACA, hexamethyldisilazane and iodotrimethylsilane at a mass ratio of 1:1.6:0.5 for 2 hours at a reaction temperature of 20°C to obtain Compound 1.

[0034] (2) Compound 1 and imidazo[1,2-b]pyridazine with a mass ratio of 1:1.5 are mixed with a solvent, the volume ratio of the compound 1 and the solvent is 1:10, and the volume ratio of the solvent is 1 : 2 mixed solution of dimethylformamide and dichloromethane, reacted for 3h, and the reaction temperature was 20°C to obtain compound 2.

[0035] (3) preparation mass concentration is 5% phosphoric acid acetonitrile solution, compound 2 is added in phosphoric acid acetonitrile solution and reacts 40min, and reaction temperature is 20 ℃, and described compound 2 and phosphoric acid acetonitrile solution volume ratio are 1:4, make ceftizole Blue intermediate crude.

[0036] (4) Th...

Embodiment 3

[0037] The preparation method of embodiment 3 cefozopran hydrochloride intermediate

[0038] (1) Using 7-ACA as the starting material, mix 7-ACA, hexamethyldisilazane and iodotrimethylsilane at a mass ratio of 1:1.8:0.7 for 3 hours at a reaction temperature of 25°C to obtain Compound 1.

[0039] (2) Compound 1 and imidazo[1,2-b]pyridazine with a mass ratio of 1:2.5 are mixed with a solvent, the volume ratio of the compound 1 and the solvent is 1:20, and the volume ratio of the solvent is 1 : 2 mixed solution of dimethylformamide and dichloromethane, reacted for 4h, and the reaction temperature was 25°C to obtain compound 2.

[0040] (3) preparation mass concentration is 7% phosphoric acid acetonitrile solution, compound 2 is added in phosphoric acid acetonitrile solution and reacts 60min, and reaction temperature is 25 ℃, and described compound 2 and phosphoric acid acetonitrile solution volume ratio are 1:6, make ceftizole Blue intermediate crude.

[0041] (4) The crude pr...

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Abstract

The invention provides a preparation method of a cefozopran hydrochloride intermediate, 7-aminocephalosporanic acid is used as a starting material to prepare the cefozopran hydrochloride intermediate 7-ACP, in the preparation method, the raw materials are reasonably proportioned, the reaction temperature is controlled to be 20-25 DEG C, and the cefozopran hydrochloride intermediate is prepared through four steps. The yield of the cefozopran hydrochloride intermediate prepared by the preparation method disclosed by the invention is as high as 96.44%, and the purity of the cefozopran hydrochloride intermediate is 99.86%.

Description

technical field [0001] The invention relates to the field of preparation of cefozopran intermediates, in particular to a preparation method of cefozopran hydrochloride intermediates. Background technique [0002] Cefazolam hydrochloride is a fourth-generation cephalosporin with a wider antibacterial spectrum and is effective against Gram-negative bacteria, Gram-positive bacteria, and Pseudomonas aeruginosa. This product has good enzyme resistance and strong penetration of bacterial cell walls. For the treatment of infections caused by sensitive bacteria. [0003] Current Chinese patent CN201010505390.X: A method for preparing an intermediate of cefazolam hydrochloride, the yield of the intermediate of cefazolam hydrochloride prepared by this method is 97%, but the purity of the finished product is also recorded CN201510381021.7: A kind of hydrochloric acid The preparation method of cefozopran intermediate 7-ACP hydrochloride also does not record the purity of the finished ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/06C07F7/10
Inventor 陆一峰韩勇
Owner HAINAN HAILING CHEMIPHARMA CORP
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