Fipronil production process

Abstract

A fipronil production process comprises the following steps that 1, concentrated sulfuric acid and sodium nitrite are used as starting raw materials, reaction is performed in a glacial acetic acid solvent to generate nitrosylsulfuric acid, then a diazo-reaction with arylamine is performed to generate arylamine diazonium salt, then a condensation reaction with dicyan ester is performed, and finally a rearrangement reaction with concentrated ammonia water is performed in an ammonia water medium to generate pyrazol; 2, the pyrazol is dissolved in an acetonitrile solvent, 13 sulfur is rapidly added at the temperature of 20 DEG C for reaction, stirring continues for 30 minutes after the temperature no longer rises, and cooling, filtration and drying are performed to obtain a sulfide product; 3, the sulfide is dissolved in N,N-dimethyl formamide, sodium formate is added and bromotrifluoromethane is introduced under the effect of a catalyst sulfur dioxide for reaction, and a fipronil sulfoxide product is obtained; 4, the fipronil sulfoxide is dissolved in a dichloromethane solvent, an oxidizing agent prepared from sulfuric acid and calcium peroxide is added to perform redox reaction, and alkaline washing, washing, crystallization, centrifugation and drying are performed to obtain a fipronil product. Compared with the prior art, the fipronil production process has the advantages that the process is reasonable and free of risk, the fipronil production process purity is improved, the production efficiency is improved, the production cost is reduced, and the environmental pollution is reduced.

Description

Technical field: [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a production process of fipronil. Background technique: [0002] Fipronil, 【chemical name】(RS)-5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethyl, is a phenylpyrazole It is an insecticide with a wide spectrum of insecticidal properties. It mainly has stomach poisoning effect on pests, and also has contact killing and certain systemic effects. Its mechanism of action is to hinder the chloride metabolism controlled by insect γ-aminobutyric acid. Important pests such as leafhoppers, planthoppers, Lepidoptera larvae, flies and Coleoptera have high insecticidal activity, and have no phytotoxicity to crops; the agent can be applied to the soil or foliar spray; applied to the soil can Effectively control corn root beetles, needleworms and cutworms; when sprayed on leaves, it has a high level of control effect on diamondback moth, cabbage butterfly...

AI Technical Summary

Problems solved by technology

[0002] Fipronil, 【chemical name】(RS)-5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethyl, is a phenylpyrazole It is an insecticide with a wide spectrum of insecticidal properties. It mainly has stomach poisoning effect on pests, and also has contact killing and certain systemic effects. Its mechanism of action is to hinder the chloride metabolism controlled by insect γ-aminobutyric acid. Important pests such as leafhoppers, planthoppers, Lepidoptera larvae, flies and Coleoptera have high insecticidal activity, and have no phytotoxicity to crops; the agent can be applied to the soil or foliar spray; applied to the soil can Effectively control corn root beetles, needleworms and cutworms; when sprayed on leaves, it has a high level of control effect on diamondback moth, cabbage butterfly, rice thrips, etc., and has a long lasting effect. The current production process is complicated and the side effects Many, low output, low efficiency of industrial production

Images