Green synthetic method for methyl-3-ethyl-4-chlorin-5-pyrazol formyl chloride
A technique for pyrazole carboxyl chloride and its synthesis method, which is applied in the field of chemical synthesis of 1-methyl-3-ethyl-4-chloro-5-pyrazole carboxyl chloride, and can solve potential safety hazards in the use process and difficulties in storage and transportation , safety hazards and other issues, to achieve the effect of no three wastes, low production cost, simple and safe operation
Inactive Publication Date: 2010-12-22
ZHEJIANG UNIV OF TECH
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Problems solved by technology
Because phosgene is a highly toxic gas that is strictly controlled and restricted internationally, there are great safety hazards in both laboratory work and industrial production; the use of thionyl chloride leads to the emission of sulfur dioxide in waste gas; trichlorochloroformate Methyl ester (diphosgene) decomposes into phosgene when encountering activated carbon, iron or organic amine, and it is difficult to store and transport. Therefore, there is a big safety hazard in the process of use
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Abstract
The invention discloses an environmental-friendly method for synthesizing 1-methyl-3-ethide-4-chlorine-5-pyrazole formyl chloride. The synthesizing method takes 1- methyl-3-ethide-4-chlorine-5- pyrazole formic acid which is shown as a formula (II) and bis (trichloromethyl) carbonate which is shown as a formula (III) as raw materials and takes organic amine as a catalyst. The raw materials and thecatalyst react sufficiently in an organic solvent at a temperature of between 20 and 80 DEG C; and the 1-methyl-3-ethide-4-chlorine-5-pyrazole formyl chloride which is shown as the formula (I) is obtained by processing the reaction fluid. Compared with prior art, the method has advanced process flow, reasonable process conditions, and cheap and available raw materials, avoids the phosgene, the Cloruro de tionilo and the trichloromethyl chloroformate, and has simple and safe operation, high reaction yield coefficient, low production cost, great implementation value and social and economical benefits and basically does not have 'three wastes'.
Description
(1) Technical field The present invention relates to a chemical synthesis method of 1-methyl-3-ethyl-4-chloro-5-pyrazole carboxylic acid chloride, 1-methyl-3-ethyl-4-chloro-5-pyrazole carboxylic acid chloride It is an important intermediate for the synthesis of new acaricide tebufenpyrad. (2) Background technology Before the present invention was made, the existing method for chemically synthesizing 1-methyl-3-ethyl-4-chloro-5-pyrazolecarbonyl chloride was from 1-methyl-3-ethyl-4-chloro-5- Synthesized from pyrazole carboxylic acid and phosgene, thionyl chloride or trichloromethyl chloroformate as raw materials, such as JP03206079, JP0469379, JP03153668, etc. Because phosgene is a highly toxic gas that is strictly controlled and restricted internationally, there are great safety hazards in both laboratory work and industrial production; the use of thionyl chloride leads to the emission of sulfur dioxide in waste gas; trichlorochloroformate Methyl ester (diphosgene) decompos...
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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/16
Inventor 谭成侠翁建全曹耀艳
Owner ZHEJIANG UNIV OF TECH
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