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Preparation method of 2,3-dichloro-6-nitroaniline

A technology of nitroaniline and trichloronitrobenzene, which is applied in the field of pesticides, can solve the problems of high reaction temperature in autoclave, cumbersome operation, and low safety, and achieve reduced production energy consumption, good reaction selectivity, and shortened reaction time Effect

Active Publication Date: 2020-09-11
常州沃腾化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN106854162A introduces that 2,3,4-trichloronitrobenzene is used as raw material, and it is prepared by ammonolysis reaction with ammonia water in an organic solvent chlorobenzene at 120-150°C in an autoclave, and the yield and purity are high. Higher, the disadvantage is that chlorobenzene has inhibitory and anesthetic effects on the central nervous system, and is irritating to the skin and mucous membranes
The disadvantages are high reaction temperature, low safety, and low yield. The product needs to be purified by column chromatography. The operation is cumbersome, and it is not easy to realize industrial production.
The disadvantage is that the reaction temperature of the autoclave is high and the safety is not high
The yield is low, the post-processing operation is cumbersome, and the production cost is high

Method used

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  • Preparation method of 2,3-dichloro-6-nitroaniline
  • Preparation method of 2,3-dichloro-6-nitroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 240g of water, 240g of 30% ammonia water, 120g of 2,3,4-trichloronitrobenzene, and 6g of p-hydroxybenzenesulfonic acid into the autoclave, start stirring, the reaction temperature is 80°C, keep the temperature for 6 hours, and the pressure is 0.3Mpa , after the reaction, cooled down to room temperature, suction filtered, washed with water, and dried to obtain 108.7g of the target product 2,3-dichloro-6-nitroaniline. The liquid phase purity is 99.5%, and the yield is 99.1%. The filtrate continues to pass through ammonia gas to the reaction concentration and then directly drops into the next batch.

Embodiment 2

[0022] Add 360g of water, 120g of 30% ammonia water, 120g of 2,3,4-trichloronitrobenzene, and 6g of p-hydroxybenzenesulfonic acid into the autoclave, start stirring, the reaction temperature is 80°C, keep the temperature for 6 hours, and the pressure is 0.4Mpa After the reaction, cool down to room temperature, filter with suction, wash with water, and dry to obtain 108.6 g of the target product 2,3-dichloro-6-nitroaniline. The liquid phase purity is 99.3%, and the yield is 99.0%. The filtrate continues to pass through ammonia gas to the reaction concentration and then directly drops into the next batch.

Embodiment 3

[0024] Add 240g of water, 480g of 30% ammonia water, 120g of 2,3,4-trichloronitrobenzene, and 6g of p-hydroxybenzenesulfonic acid into the autoclave, start stirring, the reaction temperature is 80°C, keep the temperature for 6 hours, and the pressure is 0.3Mpa After the reaction, cool down to room temperature, filter with suction, wash with water, and dry to obtain 108.9 g of the target product 2,3-dichloro-6-nitroaniline. The liquid phase purity is 99.6%, and the yield is 99.3%. The filtrate continues to pass through ammonia gas to the reaction concentration and then directly drops into the next batch.

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Abstract

The invention relates to the technical field of pesticides, in particular to a preparation method of 2,3-dichloro-6-nitroaniline. The method comprises the following steps: preparing 2,3,4-trichloronitrobenzene as a raw material, water as a solvent and a sulfur-containing compound as a catalyst, carrying out a reaction with ammonia water in a high-pressure kettle to obtain the 2,3-dichloro-6-nitroaniline. The preparation method of 2, 3-dichloro-6-nitroaniline provided by the invention is high in yield, good in reaction selectivity, high in safety, environment-friendly, low in production cost and suitable for industrial production; by adding a small amount of the sulfur-containing catalyst, a good catalytic effect can be achieved, high yield of 99% or above and selectivity of 99% or above can be finally obtained, the reaction time is greatly shortened, and the production energy consumption is reduced.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a preparation method of 2,3-dichloro-6-nitroaniline. Background technique [0002] The molecular formula of 2,3-dichloro-6-nitroaniline is C 6 h 4 Cl 2 N 2 o 2 , is an intermediate of the pesticide abenzonifen. Chinese patent CN106854162A introduces that 2,3,4-trichloronitrobenzene is used as raw material, and it is prepared by ammonolysis reaction with ammonia water in an organic solvent chlorobenzene at 120-150°C in an autoclave, and the yield and purity are high. Higher, the disadvantage is that chlorobenzene has inhibitory and anesthetic effects on the central nervous system, and is irritating to the skin and mucous membranes. It is a serious hazard to the environment and can cause pollution to water bodies, soil and the atmosphere. The reaction temperature of the autoclave is high, and the safety is not high. [0003] In the international application with the publ...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C211/52B01J31/02
CPCC07C209/10B01J31/0225B01J31/0217B01J31/0229B01J2231/4283C07C211/52
Inventor 曹伟
Owner 常州沃腾化工科技有限公司
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