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Preparation method for cefotetan disodium

A technology of cefotetan disodium and cefotetan acid, which is applied in the field of medicine, can solve the problems of dark product color, solvent residual substance content, and poor clarity, and achieve low content, low polymer and related substance content, and low raw material easy effect

Active Publication Date: 2013-05-01
CHINA MEHECO SANYANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of cefotetan disodium, to solve the problem that when the traditional method produces cefotetan disodium, the color of the product is dark, the clarity is poor, solvent residue and related substance content high problem

Method used

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  • Preparation method for cefotetan disodium
  • Preparation method for cefotetan disodium
  • Preparation method for cefotetan disodium

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preparation example Construction

[0055] The invention provides a preparation method of cefotetan disodium, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The method and application of the present invention have been described through preferred embodiments, and the relevant personnel can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention to realize and Apply the technology of the present invention.

[0056] The invention provides a preparation method of cefotetan disodium. First, take cefotetan acid and mix it with silica gel after the first salt formation, collect the first filtrate through th...

Embodiment 1

[0080] The preparation of embodiment 1 cefotetan acid

[0081] 30.00kg of 7β-amino-7α-methoxy-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl]-3-cephem-4-carboxylic acid diphenylmethyl ester Add (7-MAC) into a 500L enamel reaction kettle with 180L dichloromethane, stir for 30 minutes to dissolve it, cool down to -20°C, add 10.5kg N,N-dimethylaniline and 16.5kg bromoacetyl bromide, After reacting for 1 hour, the reaction liquid was washed successively with 30L ice water, 30L saturated potassium bisulfate solution, and 30L saturated sodium bicarbonate solution (stirring for 30 minutes during each washing, and resting for 30 minutes), layered, and the dichloromethane layer was washed with 2 kg of Dry over sodium sulfate for 60 minutes, dry the filtrate under reduced pressure at 40°C, and recover the solvent to obtain 25.2 kg of residual oil, which is 7β-bromoacetamido-7α-methoxy-3-(1-methyl-1H -5-tetrazolyl)thiomethyl-3-cephem-4-carboxylic acid benzhydryl ester;

[0082] Get 25kg of 7...

Embodiment 2

[0084] The preparation of embodiment 2 cefotetan acid

[0085] 30.00kg of 7β-amino-7α-methoxy-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl]-3-cephem-4-carboxylic acid diphenylmethyl ester Add (7-MAC) into a 500L enamel reaction kettle with 300L dichloromethane, stir for 60 minutes to dissolve it, cool down to -30°C, add 13.5kg N,N-dimethylaniline and 21.0kg bromoacetyl bromide, After reacting for 1 hour, the reaction solution was washed successively with 60L ice water, 60L saturated potassium bisulfate solution, and 60L saturated sodium bicarbonate solution (stirring for 30 minutes during each washing, and resting for 30 minutes), layered, and the dichloromethane layer was washed with 4 kg of Dry over sodium sulfate for 60 minutes, dry the filtrate under reduced pressure at 40°C, and recover the solvent to obtain 25.4 kg of residual oil, which is 7β-bromoacetamido-7α-methoxy-3-(1-methyl-1H -5-tetrazolyl)thiomethyl-3-cephem-4-carboxylic acid benzhydryl ester;

[0086] Get 25kg of...

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Abstract

The invention relates to the technical field of medicine and particularly relates to a preparation method for cefotetan disodium. In the preparation method, cefotetan acid is mixed with silica gel through a first salifying, then a first filter liquor is collected through a first filtering, the first filter liquor is mixed with EDTA and active carbon, a second filter liquor is collected through filtering, then acid-forming and crystallization are performed, and then cefotetan acid product is obtained through third filtration, collection and filter cake, as well as washing; and the cefotetan acid product is taken to be mixed with active carbon after second salifying, fourth filter liquor is collected through the fourth filtering, and then degerming and freeze drying are performed, namely the cefotetan disodium is obtained. The product prepared by using the method provided by the invention is white, is excellent in solution clarity after solution, is less in the variety of residual solvent, is low in content of relevant matters such as polymer and the like, the adopted process is simple, the raw materials are easy to access, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The technical field of medicine of the present invention relates in particular to a kind of preparation method of cefotetan disodium. Background technique [0002] Cefotetan disodium is an antibiotic with a structure as shown in formula I. It was first developed by Fujisawa Corporation of Japan in 1979 and first listed in Japan in the late 1980s. FDA Approved as New Drug on December 27, 1985 (Cefotetan Disodium Sterile Powder Injection) was launched in the United States. [0003] [0004] Formula 1 [0005] Cefotetan is by far the drug with the longest half-life among the second-generation cephalosporins (cephalosporins). Cefotetan has a strong affinity and binding to penicillin-binding protein, which blocks the synthesis of bacterial cell wall mucopeptides, thereby exerting its antibacterial activity. Because the 7th carbon atom on its β-lactam ring has a methoxyl group, it is extremely stable to β-lactamase (including penicillinase and cephal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/04C07D501/12
Inventor 张鹏飞秦坤贤刘玮朱峰李锦云
Owner CHINA MEHECO SANYANG PHARMA CO LTD
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