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Preparation method of 2,4-dichloro-3,5-dinitrobenzotrifluoride

A dinitrobenzotrifluorotoluene and nitration technology, applied in the direction of nitro compound preparation, organic compound preparation, chemical instruments and methods, etc., can solve the problems of high cost, unfavorable large-scale industrial production, low output, etc., and achieve high output High, high purity, cost-reducing effects

Inactive Publication Date: 2021-02-12
JIANGSU YONGCHUANG PHARMA TECH CO LTD
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  • Application Information

AI Technical Summary

Problems solved by technology

The existing 2.4-dichloro-3.5-dinitrobenzotrifluorotoluene production process has low output and high cost, which is not conducive to large-scale industrial production

Method used

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Examples

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Embodiment 1

[0016] A preparation method of 2,4-dichloro-3,5-dinitrobenzotrifluoride, comprising the steps of: 1) Nitrification: put measured oleum and nitric acid into a nitrification reactor and control the temperature At 40-45°C, start to add the raw material 2.4-dichlorobenzotrifluoride dropwise, complete the heat preservation for 1 hour, and then proceed to the temperature rise reaction after 1 hour, heat up to 90°C at a uniform speed in 3 hours, and heat up to 100°C in 6-7 hours, and finally use 4 The temperature is raised to 120°C in one hour, and when the temperature of the kettle reaches 120°C, the heat preservation reaction is carried out for 5 hours, wherein the pressure in the kettle of the nitration reaction is 0.01-0.02Mpa, and the sampling and analysis of mononitrate<1% is the end point; 2) Return the raw materials that the above reaction has completed In the water washing kettle, the temperature of the kettle does not exceed 120°C during water washing; after the washing is c...

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PUM

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Abstract

The invention discloses a preparation method of 2,4-dichloro-3,5-dinitrobenzotrifluoride. The method comprises the following steps: 1) nitrification: putting metered fuming sulfuric acid and nitric acid into a nitrification reaction kettle, controlling the temperature at 40-45 DEG C, starting to dropwise add a raw material 2,4-dichlorobenzotrifluoride, keeping the temperature for 1 hour, carryingout heating reaction, heating to 90 DEG C at a constant speed for 3 hours, raising the temperature to 100 DEG C within 6-7 hours, finally raising the temperature to 120 DEG C within 4 hours, keeping the temperature to react for 5 hours when the temperature of the kettle reaches 120 DEG C, and taking sampling analysis that the primary nitrate content is less than 1% as an end point; 2) returning the reacted raw materials into a water washing kettle, and separating the materials into an alkaline washing kettle after water washing is finished, wherein the temperature of the kettle does not exceed120 DEG C during water washing; 3) separating the material subjected to alkali washing into a recrystallization kettle; and 4) after the materials are crystallized, discharging and centrifuging, andthen granulating to obtain the product. The preparation method provided by the invention has the advantages of high yield and high purity, is suitable for industrial production, and reduces the cost.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediates, in particular to a preparation method of 2,4-dichloro-3,5-dinitrobenzotrifluoride. Background technique [0002] 2.4-Dichloro-3.5-dinitrotrifluorotoluene is light yellow needle-like crystal, pH is neutral, melting point is 76-78°C, boiling point is 291-294°C, flash point is 144.1°C, insoluble in water, soluble in hot ethanol , Benzene, Toluene, Acetone, main application: used as pesticide, medicine, organic synthesis intermediate. The existing 2.4-dichloro-3.5-dinitrobenzotrifluorotoluene production process has low output and high cost, which is not conducive to large-scale industrial production. Contents of the invention [0003] The object of the present invention is to provide a preparation method of 2,4-dichloro-3,5-dinitrobenzotrifluoride, so as to solve the technical problems raised in the above-mentioned background technology. [0004] In order to solve the above-m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C201/16C07C205/12
CPCC07C201/08C07C201/16C07C205/12
Inventor 孙德明杨桦罗汇吴德文花磊
Owner JIANGSU YONGCHUANG PHARMA TECH CO LTD
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