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Method for preparing 2,6-dichloro-4-trifluoromethyl phenylamine

A technology of trifluoromethylaniline and dichloride, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of hidden production safety hazards and high equipment requirements, and achieves low production cost and short reaction time. , the effect of high yield

Inactive Publication Date: 2013-11-27
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method reduces the production cost, because the ammonolysis needs to be carried out under the conditions of high temperature and high pressure, the requirements for equipment are relatively high, and there are certain hidden dangers in production safety.

Method used

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  • Method for preparing 2,6-dichloro-4-trifluoromethyl phenylamine
  • Method for preparing 2,6-dichloro-4-trifluoromethyl phenylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 200g of p-trifluoromethylaniline and 480g of dichloroethane to a 3L reaction kettle, control the temperature to 10°C, add dropwise a solution of 503g of sulfuryl chloride and 190g of dichloroethane under stirring within 3 hours, after the dropwise addition is completed, in Continue to react at 50°C for 2 hours. After the reaction is completed, cool down, wash with water, and wash with saturated sodium carbonate aqueous solution to remove the inorganic salts. After the organic phase is concentrated to remove the solvent, rectify to obtain 2,6-dichloro-4-trifluoromethylaniline 144g.

Embodiment 2

[0025] Add 200g of p-trifluoromethylaniline and 720g of dichloroethane to a 3L reactor, control the temperature to 25°C, add dropwise a mixed solution of 496g of sulfonyl chloride and 190g of dichloroethane under stirring within 3 hours, after the dropwise addition is completed, in Continue to react at 60°C for 4 hours, lower the temperature, wash with water and saturated aqueous sodium carbonate solution to remove inorganic salts, concentrate the organic phase to remove the solvent, and rectify to obtain 160 g of 2,6-dichloro-4-trifluoromethylaniline.

Embodiment 3

[0027] Add 200g of p-trifluoromethylaniline and 700g of N,N-dimethylformamide to a 3L reactor, control the temperature to 40°C, add a mixed solution of 485g of sulfuryl chloride and 190g of dichloroethane dropwise with stirring within 3 hours, dropwise After the addition, continue the reaction at 70°C for 1 hour, lower the temperature, wash with water, and wash with saturated sodium carbonate aqueous solution to remove the inorganic salts, concentrate the organic phase to remove the solvent, and rectify to obtain 2,6-dichloro-4-trifluoromethyl Aniline 120g.

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Abstract

The invention relates to a method for preparing 2,6-dichloro-4-trifluoromethyl phenylamine. The method is characterized by comprising the following steps of: adding p-trifluoromethylaniline into a corresponding solvent; dripping a certain amount of sulfonyl chloride by controlling a reaction temperature of 0 DEG C to 70 DEG C; contiguously reacting for 1 to 15 hours by controlling the reaction temperature to 30 DEG C to 70 DEG C after the dripping of the sulfonyl chloride; removing an inorganic salt from the mixture in a water washing manner after the reaction; and performing decompression and rectification after the concentration of an organic phase, thereby obtaining the corresponding 2,6-dichloro-4-trifluoromethyl phenylamine, wherein the adopted solvent is a mixed solvent selected from any one or two and more than two materials from N,N-dimethyl formamide, ethyl acetate, dichloromethane, trichloromethane, carbon tetrachloride and dichloroethane. The method has the advantages of being simple in process, easy to operate, short in reaction time, high in yield, low in production cost and easy in industrial production. Thus, the method is an environment-friendly chemical process which has a good industrial application prospect.

Description

technical field [0001] The invention relates to a new method for preparing 2,6-dichloro-4-trifluoromethylaniline, belonging to the technical field of chemical material preparation. The method is applicable to the occasion of synthesizing 2,6-dichloro-4-trifluoromethylaniline by reacting p-trifluoromethylaniline and sulfonyl chloride as raw materials under normal pressure. Background technique [0002] 2,6-Dichloro-4-trifluoromethylaniline is an important pesticide synthesis intermediate, mainly used to synthesize fluorine-containing organic pesticides such as fipronil. Fipronil is currently the preferred chemical pesticide for pollution-free agricultural and sideline products. It has the characteristics of high efficiency, long-acting, broad-spectrum, low dosage, safety to humans, animals and the environment, and mild to natural enemies of insects and beneficial organisms. It has a broad market prospect. The main preparation methods of 2,6-dichloro-4-trifluoromethylaniline ...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/74
Inventor 郑龙生李付香褚吉成
Owner JIANGSU FENGHUA CHEM IND
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