Method for synthesizing trichlorine methoxyl chlorobenzene and trichlorine methoxyl phenylamine

A technology of trichloromethoxychlorobenzene and chlorotrichloromethoxybenzene, which can be applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc. Yield decline and other problems, to achieve high industrial value, cheap and easy to obtain raw materials, less by-products

Active Publication Date: 2014-05-07
阜新汉道化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other above-mentioned solvents have problems such as separation difficulties; rising industrial costs; many by-products and decreased reaction yields
Trifluoromethoxyaniline is mostly produced by nitration and reduction of trifluoromethoxybenzene in the industry, but a large amount of waste acid, waste water and isomers will be produced during the nitration process, causing environmental pollution and difficulty in product separation

Method used

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  • Method for synthesizing trichlorine methoxyl chlorobenzene and trichlorine methoxyl phenylamine
  • Method for synthesizing trichlorine methoxyl chlorobenzene and trichlorine methoxyl phenylamine
  • Method for synthesizing trichlorine methoxyl chlorobenzene and trichlorine methoxyl phenylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] In a 500mL reaction flask, add p-trifluoromethylbenzene (200g, 145ml), 2 grams of dimethyl azobisisobutyrate and 2 grams of phosphorus trichloride in sequence, raise the temperature to 60°C, and turn on the mercury lamp for the reaction The solution was illuminated, and chlorine gas was introduced into the bottle at a rate of 20ml / s. Simultaneously, 80g (0.56mol) of p-chloroanisole was added dropwise, and the dripping was completed in 1 hour. After the dropwise addition, continue to maintain the reaction at 70-80°C. The end point of the reaction is tracked and detected by GC. The mass content of dichlorobenzyl <0.5% is the end point of the reaction. At this time, the reaction time is 5 hours. Stop feeding chlorine gas, and then carry out air purging. The solvent in the reaction solution was removed by distillation (ceramic corrugated packing) to obtain 135 grams of the target product (4-chlorotrichloromethoxybenzene), with a content of 95.2% and a yield of 93%.

[0056]...

Embodiment 2

[0059] Into a 500 mL reaction flask, add p-trifluoromethylbenzene (400 g, 285 ml), 2 g of dimethyl azobisisobutyrate and 2 g of phosphorus trichloride in sequence, and the rest of the operations are the same as in Example 1. After removing the solvent from the reaction solution, 136 g of the target product (4-chlorotrichloromethoxybenzene) was obtained, with a content of 95.4% and a yield of 93.9%.

Embodiment 3

[0061] Into a 500 mL reaction flask, add p-trifluoromethylbenzene (480 g, 345 ml), 2 g of dimethyl azobisisobutyrate and 2 g of phosphorus trichloride in sequence, and the rest of the operations are the same as in Example 1. After removing the solvent from the reaction solution, 136 g of the target product (4-chlorotrichloromethoxybenzene) was obtained, with a content of 95.5% and a yield of 94.0%.

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Abstract

The invention discloses a method for synthesizing trichlorine methoxyl chlorobenzene and trichlorine methoxyl phenylamine. One of 4-chlorine trichlorine methoxyl benzene, 3-chlorine trichlorine methoxyl benzene and 2-chlorine trichlorine methoxyl benzene is synthesized by performing photochlorination reaction on one of 4-chloroneb, 3-chloroneb and 2-chloroneb serving as a raw material and chlorine in a solvent under the action of a catalyst. The corresponding 4-chlorine trichlorine methoxyl benzene, the 3-chlorine trichlorine methoxyl benzene and the 2-chlorine trichlorine methoxyl benzene are obtained by separating the solvent. One of the 4-chlorine trichlorine methoxyl benzene, the 3-chlorine trichlorine methoxyl benzene and the 2-chlorine trichlorine methoxyl benzene is mixed with hydrogen fluoride, and the mixture is fluorinated and ammoniated and then is rectified to obtain the corresponding 4-trichlorine methoxyl phenylamine, the 3-trichlorine methoxyl phenylamine and the 2-trichlorine methoxyl phenylamine. The method has the characteristics of simple operation, mild reaction condition, no three-waste emission, easiness in separation of a product and the solvent and the like, and forbidden chemical substances required by the international and national environment protection organizations are not used.

Description

technical field [0001] The invention discloses a method for synthesizing trichloromethoxychlorobenzene and trifluoromethoxyaniline. Using methoxychlorobenzene as raw material, the photochlorination reaction with chlorine gas under the action of solvent and catalyst is used to synthesize trichloromethoxychlorobenzene. Trichloromethoxychlorobenzene was obtained after separation of the solvent. After fluorination and ammoniation, trifluoromethoxyaniline is obtained. Compared with the reported production methods, the present invention has the characteristics of simple operation, mild reaction conditions, easy separation of products, no isomers, and environmental protection. Background technique [0002] With the advancement of science, new products and materials with high performance, high quality and high technology content are constantly coming out in various fields. important intermediates. [0003] The fluorine in the fluorine-containing organic intermediate has a small a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/247C07C41/22C07C217/84C07C213/02
CPCC07C41/22C07C213/02C07C43/225C07C217/84
Inventor 刘军刘影赵名道台立民刘东宇倪国昊谢雨杨领军
Owner 阜新汉道化工有限责任公司
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