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Method for synthesis of 2,4-dichloro-3,5-dinitro trifluorotoluene in micro reactor

A technology of dinitrotrifluorotoluene and dichlorotrifluorotoluene is applied in the field of organic fine synthesis, and achieves the effects of convenient operation, reduction of raw material storage, transportation and reaction risks

Inactive Publication Date: 2017-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There is no reference in the literature on the synthesis of 2,4-dichloro-3,5-dinitrobenzotrifluoride in a microreactor

Method used

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  • Method for synthesis of 2,4-dichloro-3,5-dinitro trifluorotoluene in micro reactor

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Experimental program
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Effect test

Embodiment 1

[0023] The molar ratio of 95% nitric acid-98% sulfuric acid is 1:4, and the molar ratio of 2,4-dichlorotrifluorotoluene is 1.05. The two streams enter the microchannel for reaction, the residence time is 120s, and the reaction temperature is 140°C. The conversion rate of 2,4-dichlorobenzotrifluoride was 97.2%, and the yield of 2,4-dichloro-3,5-dinitrobenzotrifluoride was 22.6%.

Embodiment 2

[0025] The molar ratio of 95% nitric acid-98% sulfuric acid is 1:5, and the molar ratio of 2,4-dichlorotrifluorotoluene is 1.05. The two streams enter the microchannel for reaction, the residence time is 120s, and the reaction temperature is 150°C. The conversion rate of 2,4-dichlorobenzotrifluoride was 97.7%, and the yield of 2,4-dichloro-3,5-dinitrobenzotrifluoride was 30.8%.

Embodiment 3

[0027] The molar ratio of 95% nitric acid-98% sulfuric acid is 1:6, and the molar ratio of 2,4-dichlorotrifluorotoluene is 1.05. The two streams enter the microchannel for reaction, the residence time is 150s, and the reaction temperature is 160°C. The conversion rate of 2,4-dichlorobenzotrifluoride was 98.1%, and the yield of 2,4-dichloro-3,5-dinitrobenzotrifluoride was 40.7%.

[0028] In the above embodiment, the reaction time is only about 200s, the operation is simple and the effect is good.

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Abstract

The invention relates to a method for synthesis of 2,4-dichloro-3,5-dinitro trifluorotoluene in a micro reactor, that is to say, in the micro reactor, a raw material 2,4-dichloro trifluorotoluene and a nitrating agent composed of concentrated sulfuric acid and concentrated nitric acid are introduced in proportion for synthesis of 2,4-dichloro-3,5-dinitro trifluorotoluene. The method is simple, and is good in effect; compared with a traditional method, the method greatly shortens the reaction time (which is reduced from 96 h to about 200 s), improves the production efficiency, and has the 2,4-dichloro-3,5-dinitro trifluorotoluene yield of 40%.

Description

technical field [0001] The invention belongs to the field of fine organic synthesis, and relates to a method for synthesizing 2,4-dichloro-3,5-dinitrobenzobenzotrifluoride in a microreactor, that is, in the microreactor, raw materials 2 , 4-dichlorobenzotrifluoride and nitrating agent to synthesize 2,4-dichloro-3,5-dinitrobenzotrifluoride. Background technique [0002] 2,4-dichloro-3,5-dinitrobenzotrifluoride is an organic intermediate, commonly used in the synthesis of pesticides and medicines. At present, there is no relevant synthesis technology in domestic literature, and there are few reports in foreign literature. People such as Hori Hitoshi mentioned in "Design and Synthesis of New Mitochondiral Cytotoxin N-Thiadiazolyanilines that Inhibit Tumor Cell Growth" that 50% concentration of oleum and fuming nitric acid are mixed as nitrating agent, and 2,4-dichlorotri Fluorotoluene was stirred and reacted at 80°C for 96 hours to synthesize 2,4-dichloro-3,5-dinitrobenzotrif...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08
Inventor 任磊李秀清黄伟何志勇金钢
Owner CHINA PETROLEUM & CHEM CORP
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