Preparation method for fluazinam

A technology based on trifluoromethylpyridine and pyridyl, applied in the field of compound synthesis, can solve the problems of limited range of solvent selection, increase of waste water treatment cost, increase of alkali removal workload, etc., to suppress hydrolysis side reactions and benefit environmental protection , improve the effect of selectivity
CN108929264AInactive Publication Date: 2018-12-04江苏禾裕泰化学有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
江苏禾裕泰化学有限公司
Publication Date
2018-12-04
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a preparation method for fluazinam. The method comprises the following steps: performing a reaction on 2-amino-3-chloro-5-trifluoromethylpyridine and 2,4-dichloro-3,5-dinitrobenzotrifluoride in the presence of a first organic solvent, an alkali and a catalyst at a specified reaction temperature to obtain a reaction mixture; and performing post treatment to obtain purified 3-chloro-N-(3-chloro-5-trifluoromethyl-2-pyridinyl)-alpha-alpha-alpha-trifluoro-2,6-dinitro-p-toluidine as a reaction product from the reaction mixture, wherein a catalyst is a phase transfer catalyst.According to the method disclosed by the invention, the phase transfer catalyst is added to the reaction, the reaction temperature is reduced, so that selectivity of the reaction is improved, an occurrence of a hydrolysis side reaction is inhibited, and a yield of the product is improved; and further, in the post treatment of the product, the alkali and the formed salt are removed by filtration and neutralization without water washing, and the alkali can be reused, so that generation of wastewater and waste of resources are reduced.
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Description

technical field

[0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of fluazinam. Background technique

[0002] Fluazinamine (chemical name: 3-chloro-N-(3-chloro-5-trifluoromethyl-2-pyridyl)-α,α,α-trifluoro-2,6-dinitro-p-methyl Aniline; English name: fluazinam; trade name: SHIRLAN, IKF-1216) is a new type of substituted aniline broad-spectrum fungicide developed by Japan Ishihara Industry Co. It also has good activity on diseases caused by fungi such as Phytophthora, Phytophthora, Plasmodium, Sclerotinia and Scabella.

[0003] At present, the synthetic method of fluazinam mainly adopts compound A (2-amino-3-chloro-5-trifluoromethylpyridine) and compound B (2,4-dichloro-3,5-dinitrotrifluoro Toluene) under the effect of alkali and solvent, prepare fluazinam, concrete reaction equation is as follows:

[0004]

[0005] In this synthesis method, due to the presence of water in the solvent, compound B (...

Claims

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