Synthesis technology of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole

Abstract

The invention provides a synthesis technology of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole. The technology includes the following steps that firstly, nitrosyl sulfuric acid is added into a reaction kettle and stirred, and a mixed solution of 4-amino-3,5-dichlorobenzotrifluoride and acetic acid is added dropwise, and a heavy nitrogen solution is obtained; secondly, water and ethyl 2,3-dicyanopropionate are added into another reaction kettle, the heavy nitrogen solution is added, the mixture stands still and layers, the upper layer is a waste alkaline water layer, and the bottom layer is a material layer; thirdly, chlorobenzene is extracted; fourthly, waste alkaline water is added into an ammoniation kettle and cooled, and the material layer and the chlorobenzene extract are added; fifthly, ammonia water is added, heat is preserved, the mixture stands still and layers, the upper layer is reused, and the bottom layer is a material layer; sixthly, water is added to wash the material layer, stirring is conducted, and the mixture stands still and layers; seventhly, material liquid is conveyed to a crystalization kettle, stirred, cooled, centrifuged, spun and dried to obtain the finished product. The process route is simple, a synthesis device is simple, the synthesis raw materials and the synthesis technology are environmentally friendly, synthesis cost is low, the product yield is high, production cost is effectively reduced, energy conservation and consumption reduction are achieved, and cost is reduced.

Description

technical field [0001] The invention relates to a synthesis process of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole. Background technique [0002] 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole is called pyrazole ring for short. The pure product is a white crystalline solid, and the industrial product is a light yellow-brown solid, with a melting point of 141-142°C. It is soluble in methanol, ethanol, acetone, dichloroethane and ethyl acetate. intermediate. [0003] The quality of its synthesis effect and the level of synthesis efficiency will directly have a major impact on the insecticidal effect of fipronil and ethiprole. [0004] Fipronil is a phenylpyrazole insecticide with a wide insecticidal spectrum. It mainly has gastric toxicity to pests, and also has contact killing and certain systemic effects. Its mechanism of action is to hinder insect γ-aminobutyric acid Controlled chloride metabolism, so it has high insecticidal activi...

AI Technical Summary

Problems solved by technology

However, the intermediate considered by the patent is 5-amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-(trifluoromethylthio)-1H-pyrazole -3-carbonitrile is prepared by alkylthiolation of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole according to the present invention, The preparation method for 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole is not mentioned