Preparation method of 3-difluoro-methyl pyrazole-4-carboxylic acid and 3-trifluoro-methyl pyrazole-4-carboxylic acid

A technology of methylpyrazole and difluoromethyl is applied in the field of preparation of 3-difluoromethylpyrazole-4-carboxylic acid and 3-trifluoromethylpyrazole-4-carboxylic acid, and can solve the problem of reaction Harsh equipment requirements, poor selectivity, waste of fluorine sources, etc.
CN102718712BActive Publication Date: 2015-04-29LANZHOU CHEMSPECWEIER CHEM CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
LANZHOU CHEMSPECWEIER CHEM CO LTD
Publication Date
2015-04-29

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Abstract

The invention provides a preparation method of 3-difluoro-methyl-1H-methyl pyrazole-4-carboxylic acid shown in the formula (I) or 3-trifluoro-methyl-1H-methyl pyrazole-4-carboxylic acid shown in the formula (II), and the method comprises the following steps of: (a) providing a 3-polyfluoro methyl-1H-pyrazole-4-nitrile group shown in the formula (VII); and (b) under the condition of participation of acid or alkaline, carrying out hydrolysis reaction on the 3-polyfluoro methyl-1H-pyrazole-4-nitrile group shown in the formula (VII), thus obtaining the 3-difluoro-methyl-1H-methyl pyrazole-4-carboxylic acid shown in the formula (I) or 3-trifluoro-methyl-1H-methyl pyrazole-4-carboxylic acid shown in the formula (II).
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Description

technical field

[0001] The present invention relates to the preparation method of compound 3-difluoromethyl-1H-methylpyrazole-4-carboxylic acid and compound 3-trifluoromethyl-1H-methylpyrazole-4-carboxylic acid. Background technique

[0002] Pyrazole amide structure is an important species of fungicides. 3-Difluoromethyl-1H-methylpyrazole-4-carboxylic acid is a common intermediate of the fungicide Bixafen developed by Bayer and Isopyrazam developed by Syngenta; 3-trifluoromethyl-1H-methyl Pyrazole-4-carboxylic acid is an intermediate of the fungicide penthiopyrad developed by Mitsui Chemicals.

[0003] In the prior art, Mitisui's patented method (US2010016612) uses difluoroacetic acid or trifluoroacetic acid as a raw material, under the action of oxalyl chloride or triphosgene, undergoes an addition and elimination reaction with 3-aminoacrylonitrile, and then reacts with methyl hydrazine The reaction proceeds to cyclization and finally hydrolysis to obtain the correspondin...

Claims

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