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A method for continuously synthesizing 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile in a microreactor

A technology of trifluoromethylpyrrole and p-chlorophenyl, which is applied in the field of continuous synthesis of 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile in a microreactor, can solve the problems that are not completely solve other problems

Active Publication Date: 2020-07-10
湖南海利常德农药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Micro-reaction technology is a new type of chemical technology that replaces traditional batch reactors with micro-pipe reactors based on continuous flow. It has the advantages of good mixing performance and high safety. However, ordinary micro-reactors are used for 2-p-chlorobenzene The bromination synthesis of base-5-trifluoromethylpyrrole-3-carbonitrile does not completely solve the shortcomings of the above-mentioned general batch bromination method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for continuously synthesizing 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile in a microreactor, comprising the following steps:

[0023] (1) Preparation solution: Mix 27.3g 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile with 518.7g methanol to obtain 2-p-chlorophenyl-5-trifluoromethylpyrrole-3- Nitrile solution. Mix 8g of bromine with 392g of methanol to obtain a bromine solution. Mix 5.7g of 30% hydrogen peroxide with 334.3g of methanol to obtain a hydrogen peroxide solution.

[0024] (2) be 5.46g / min, 4.0g / min with feed rate respectively, the 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile solution that prepares in step (1) and bromine The solution is simultaneously and continuously pumped into the first reaction module of the microreactor for reaction, and the temperature of each reaction module is controlled to be 50°C. After the resulting mixed solution flows through the third reaction module of the microreactor, the ...

Embodiment 2

[0026] A method for continuously synthesizing 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile in a microreactor, comprising the following steps:

[0027](1) Preparation solution: Mix 27.3g 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile with 245.7g methanol to obtain 2-p-chlorophenyl-5-trifluoromethylpyrrole-3- Nitrile solution. Mix 8g of bromine with 152g of methanol to obtain a bromine solution. Mix 5.7g of 30% hydrogen peroxide with 164.3g of methanol to obtain a hydrogen peroxide solution.

[0028] (2) be 2.73g / min, 1.6g / min with the feed rate respectively, the 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile solution that prepares in step (1) and bromine The solution is continuously pumped into the first reaction module of the microreactor to react, and the temperature of each reaction module is controlled to be 64°C. pump the hydrogen peroxide solution prepared in step (1) into the microreactor, react the mixed solution with the hydro...

Embodiment 3

[0030] A method for continuously synthesizing 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile in a microreactor, comprising the following steps:

[0031] (1) Preparation solution: Mix 27.3g 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile with 109.2g methanol to obtain 2-p-chlorophenyl-5-trifluoromethylpyrrole-3- Nitrile. Mix 8g of bromine with 72g of methanol to obtain a bromine solution. Mix 5.7g of 30% hydrogen peroxide with 28.3g of methanol to obtain a hydrogen peroxide solution.

[0032] (2) Be 1.37g / min, 0.8g / min with the feed rate respectively, the 2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile solution that prepares in step (1) and bromine The solution is simultaneously and continuously pumped into the first reaction module of the microreactor for reaction, and the temperature of each reaction module is controlled at 64°C. After the resulting mixed solution flows through the fifth reaction module of the microreactor, the feed rate ...

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Abstract

The invention discloses a method for continuous synthesis of 4-bromo-2-(p-chlorophenyl)-5-(trifluoromethyl) pyrrole-3-carbonitrile through a microreactor. The method comprises the steps that a 2-(p-chlorophenyl)-5-(trifluoromethyl) pyrrole-3-carbonitrile solution and a bromine solution are simultaneously and continuously added into the microreactor for reaction, an obtained mixed solution flows through two or more reaction modules in the microreactor and then are introduced into a hydrogen peroxide solution in the microreactor for reaction and distillation, and thus continuous preparation of the 4-bromo-2-(p-chlorophenyl)-5-(trifluoromethyl) pyrrole-3-carbonitrile through the microreactor is achieved. According to the method, the whole technological procedure is simple, the process is continuous, the method has the characteristics of high efficiency, low energy consumption, no pollution and the like, the method is an efficient and environmental-friendly continuous synthesis technologyprocess of the 4-bromo-2-(p-chlorophenyl)-5-(trifluoromethyl) pyrrole-3-carbonitrile and is suitable for large-scale continuous preparation, and industrial utilization is facilitated.

Description

technical field [0001] The invention relates to a method for continuously synthesizing 4-bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile with a microreactor. Background technique [0002] 4-Bromo-2-p-chlorophenyl-5-trifluoromethylpyrrole-3-carbonitrile is an important intermediate of arylpyrrole nitrile insecticides and acaricides chlorfenapyr and chlorfenapyr, the main synthesis method It is synthesized by bromination reaction of 2-p-chlorophenyl-5-trifluoromethyl-pyrrole-3-carbonitrile and bromine. Batch synthesis is generally adopted in industry. This process has the advantages of simple operation and low cost, but at the same time, it has disadvantages such as slow reaction speed, excessive raw material bromine required, more waste acid produced, and greater safety risks. [0003] Micro-reactor, that is, micro-channel reactor, generally refers to a small reaction system manufactured by micro-processing and precision processing technology. "Micro" means th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/34
CPCC07D207/34
Inventor 刘源刘卫东杜升华兰世林王艳丽孔晓红
Owner 湖南海利常德农药化工有限公司
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