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Preparation method of cefoperazone intermediate 7-TMCA

A technology of cefoperazone and 7-ACA, which is applied in the field of preparation of 7-TMCA, can solve the problems of environmental hazards, water pollution, and the cost of treatment of a large amount of polluted water, and achieve easy transportation, avoid energy waste, and shorten drying time Effect

Inactive Publication Date: 2012-08-08
HEILONGJIANG HAOYUN FINE CHEM
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Problems solved by technology

Sulfurous acid needs to be added in the washing process. Sulfuric acid is harmful to the environment and will also cause certain pollution to the water body, and it requires a lot of cost for the treatment of polluted water bodies, and then provides a preparation of cefoperazone intermediate 7-TMCA method

Method used

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Embodiment Construction

[0016] The present invention will be described in further detail below: the present embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation is provided, but the protection scope of the present invention is not limited to the following examples.

[0017] A kind of preparation method of cefoperazone intermediate 7-TMCA involved in the present embodiment, its steps are:

[0018] 1. Add dimethyl carbonate and boron trifluoride dimethyl carbonate complex to the first 1L reaction bottle A, start stirring, and cool down;

[0019] 2. When the temperature drops to 10-15°C, put methylmercaptotetrazolium into the bottle and stir for 10-30 minutes to completely dissolve it;

[0020] 3. Put 7-ACA into the first 1L reaction bottle A (the molecular formula of 7-ACA is C 10 h 12 N 2 o 5 S, the molecular weight is 272.28. The chemical name of 7-ACA is 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid...

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Abstract

The invention provides a preparation method of cefoperazone intermediate 7-TMCA. The preparation method comprises the following steps of: adding a boron trifluoride dimethyl carbonate complex and dimethyl carbonate into a first 1L reaction bottle A; starting to stir; throwing methyl mercaptotetrazole into the bottle when the temperature is reduced to 10-15 DEG C; stirring for 10-30 minutes to fully dissolve the methyl mercaptotetrazole; transferring reaction solution from the first 1L reaction bottle A into a second 1L reaction bottle B in which de-ionized water is held; and drying under a vacuum condition at 80 DEG C for 3-4 hours and taking out. According to the preparation method, the dimethyl carbonate is used as a solvent in place of acetonitrile, the boron trifluoride dimethyl carbonate complex is used as a catalyst in place of a boron trifluoride acetonitrile complex, and the dimethyl carbonate is non-toxic, has similar physical property to that of water, is safe and convenient to use, has less pollution and is easy to transport. An obtained product has a better crystal form and is not required to be crushed in a drying step; and the drying time of the product can be shortened.

Description

technical field [0001] The invention relates to a preparation method of cefoperazone intermediate 7-TMCA, belonging to the technical field of 7-TMCA preparation. Background technique [0002] In the preparation method of existing cefoperazone intermediate 7-TMCA, usually with acetonitrile as solvent, boron trifluoride acetonitrile complex as catalyst, acetonitrile has certain toxicity, safety and convenience are slightly worse in use, and have pollute. The crystal form of the product obtained by using acetonitrile as a solvent is not very good, and the product needs to be pulverized after drying, and the product takes a long time to dry, and the energy waste in the drying process is relatively serious. Sulfurous acid needs to be added in the washing process. Sulfurous acid is harmful to the environment and will also cause certain pollution to water bodies, and requires a lot of costs for the treatment of polluted water bodies. Contents of the invention [0003] The purpo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18
Inventor 李雪李晴孙晓凤朱云波龚真固梁园园
Owner HEILONGJIANG HAOYUN FINE CHEM
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