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Method for producing 2,6-dichloro-4-trifluoromethylaniline

A technology of trifluoromethylaniline and trichlorobenzotrifluoride, which is applied to the preparation of amino compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult purification of products, corrosion of equipment, expensive raw materials, etc., and achieve reduction Low production cost, low equipment corrosion, and easy industrialization

Active Publication Date: 2008-04-23
SHANGHAI HETENG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Document EP599,704 discloses to use p-chlorobenzotrifluoride or 3,4-dichlorobenzotrifluoride as raw material to prepare N,N-dimethyl-2,6-dichloro-p-trifluoromethylaniline and then chlorinate Process for obtaining 2,6-dichloro-p-trifluoromethylaniline, which has the disadvantage of the pressure in the autoclave for the preparation of the starting material N,N-dimethyl-2,6-dichloro-p-trifluoromethylaniline It is difficult to control and may even explode out of control. In addition, the equipment is severely corroded during chlorination, and the product is difficult to purify
[0006] In summary, the above methods are either expensive in raw materials, or have great disadvantages, so it is necessary to find another preparation method

Method used

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  • Method for producing 2,6-dichloro-4-trifluoromethylaniline
  • Method for producing 2,6-dichloro-4-trifluoromethylaniline

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 200 grams of 3,4,5-trichlorobenzotrifluoride, 200 grams of potassium fluoride and 500 milliliters of sulfolane into a 1L three-neck reaction flask equipped with a stirrer, reflux condenser and temperature, then heat to 190°C and keep warm After stirring for 20 hours, it was cooled to 100°C.

[0021] 200 g of crude product (containing about 10% sulfolane) were distilled out under a pressure of 0.01 MPa. Then the temperature was raised to 150° C. to recover sulfolane under reduced pressure (it can be directly used in the next batch of reactions).

[0022] 200 g of crude product 3,5-dichloro-4-fluorobenzotrifluoride was directly used in the next step of ammoniation reaction.

Embodiment 2

[0024] Add 200 grams of crude product 3,5-dichloro-4-fluorobenzotrifluoride and 300 milliliters (0.892 g / ml) of 30% ammonia water in Example 1 into a 1L autoclave, heat up to 150° C., and then keep stirring for 24 hours. Cooling, discharging, layering, separate the lower oil layer (the water layer can be used for the next batch of reactions); the oil layer is subjected to vacuum distillation to obtain 153 grams (97%) of 2,6-dichloro-p-trifluoromethyl Aniline (melting point: 32-34 degrees).

Embodiment 3

[0026] Add 100 grams of 3,5-dichloro-4-fluorobenzotrifluorotoluene crude product and 30 grams of liquid ammonia prepared by the method in Example 1 into a 300-ml autoclave, then heat up to 140 ° C, then keep stirring for 6 hours, and then remove the residual ammonia Discharge (water absorption), cool the discharge, and rectify under reduced pressure to obtain 78 grams (97.4%) of 2,6-dichloro-p-trifluoromethylaniline (melting point: 32-34 degrees).

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Abstract

The present invention discloses 2, 6-dichloro-p-trifluoro methyl aniline preparing process, which includes the first reaction of 3, 4, 5-trichloro trifluoro toluene and fluoride salt in solvent to produce 3, 5-dichloro-4-fluoro trifluoro toluene, and the subsequent reaction of 3, 5-dichloro-4-fluoro trifluoro toluene and liquid ammonia or ammonia water to obtain 2, 6-dichloro-p-trifluoro methyl aniline. The process has 3, 4, 5-trichloro trifluoro toluene as the side product from p-chloro trifluoro toluene producing process adopted, lowered production cost, no use of acid matter and less corrosion of the equipment.

Description

technical field [0001] The invention relates to a preparation method of 2,6-dichloro-p-trifluoromethylaniline. Background technique [0002] 2,6-Dichloro-p-trifluoromethylaniline is a chemical intermediate of medicine and pesticide, which is widely used in the fields of medicine and pesticide. At present, there are mainly the following preparation methods: [0003] The most direct method is, p-trifluoromethylaniline reacts with chlorine to generate 2,6-dichloro-p-trifluoromethylaniline, such as documents EP34402, EP639,556, but the preparation process of p-trifluoromethylaniline is complicated and the operation Conditions are harsh and products are expensive. [0004] Document Fr1,545,142 discloses a method for preparing 2,6-dichloro-p-trifluoromethylaniline by hydrolysis of 2,6-dichloro-p-trifluoromethylbenzene isocyanate in concentrated sulfuric acid, but in fact 2,6 -Dichloro-p-trifluoromethylbenzene isocyanate is more difficult to prepare than 2,6-dichloro-p-trifluoro...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/10
Inventor 施冠成吉景顺
Owner SHANGHAI HETENG FINE CHEM
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