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Preparation method of m-nitrobenzotrifluoride

A technology of nitrobenzotrifluoride and trifluorotoluene, which is applied in the field of preparation of m-nitrobenzotrifluoride, can solve the problems of tediousness and post-explosion treatment, achieve low risk, reduce violent heat release, and solve cumbersome post-treatment Effect

Active Publication Date: 2020-08-07
BEIJING GREENCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of m-nitrobenzotrifluoride, to overcome the deficiencies of the existing technology, to solve the problems of possible explosion in the reaction process and complicated post-treatment, and to obtain high-yield, high-quality m-nitrobenzotrifluoride. Trifluorotoluene

Method used

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  • Preparation method of m-nitrobenzotrifluoride
  • Preparation method of m-nitrobenzotrifluoride

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[0024] The invention provides a method for preparing m-nitrobenzotrifluoride, which uses an organic solvent to participate in the preparation of m-nitrobenzotrifluoride.

[0025]

[0026] The preparation method of m-nitrobenzotrifluoride of the present invention comprises: adding trifluorotoluene shown in formula (I), organic solvent and concentrated sulfuric acid into the reaction vessel, under stirring, temperature control 30~40 ℃, dripping Smoked nitric acid, insulation reaction for 6-10 hours, after the reaction finishes, let stand to separate the liquids, the organic phase is adjusted to be alkaline with alkaline aqueous solution, the organic phase is desolvated, and finally carry out decompression distillation to obtain the formula (II) of m-nitrobenzotrifluoride.

[0027] Specifically, the organic solvent is usually a chlorinated non-polar solvent, such as dichloroethane, carbon tetrachloride, and the like. The molar ratio of trifluorotoluene to the organic solvent ...

Embodiment 1

[0039] Add 1kg of industrially pure trifluorotoluene (commercially available), 1L of dichloroethane and 336g of 98% concentrated sulfuric acid into the reaction flask, and under stirring, add 475g of fuming nitric acid dropwise at 30-40°C, dropwise After the addition, stir for 8 hours at 30-40°C, let stand, separate the liquid, remove the acid phase, wash the organic phase with aqueous sodium hydroxide solution to alkalinity, then carry out precipitation of the organic phase, and finally carry out subtractive evaporation to obtain Light yellow oily liquid m-nitrobenzotrifluoride 915g, the calculated yield is 69.8%, the purity of m-nitrobenzotrifluoride obtained by gas chromatography is 99.0%.

Embodiment 2

[0041] Add 1kg of industrially pure trifluorotoluene (commercially available), 1L of dichloroethane and 470g of 98% concentrated sulfuric acid into the reaction flask, and under stirring, add 475g of fuming nitric acid dropwise at 30-40°C. After the addition, stir for 8 hours at 30-40°C, let stand, separate the liquid, remove the acid phase, wash the organic phase with aqueous sodium hydroxide solution to alkalinity, then carry out precipitation of the organic phase, and finally carry out subtractive evaporation to obtain Light yellow oily liquid m-nitrobenzotrifluoride 1205g, the calculated yield is 92.0%, the purity of m-nitrobenzotrifluoride obtained by gas chromatography is 99.0%.

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Abstract

The invention relates to a preparation method of m-nitrobenzotrifluoride. The method includes carrying out nitration reaction on trifluorotoluene, concentrated sulfuric acid and nitric acid in an organic solvent; specifically, stirring trifluorotoluene, an organic solvent and concentrated sulfuric acid under the condition that the temperature is controlled to be 30-40 DEG C, adding fuming nitric acid is dropwise, performing a heat preservation reaction for 6-10 h; after the reaction is completed, standing and performing liquid separation, adjusting the pH of an organic phase to be alkaline with an alkaline aqueous solution, performing desolvation on the organic phase, and finally performing reduced pressure distillation to obtain m-nitrotrifluorotoluene. According to the invention, dichloroethane, carbon tetrachloride and other chlorinated non-polar solvents are used as reaction solvents for nitration reaction, so violent heat release in the nitration reaction process is reduced, the reaction conditions are mild, and the safety is improved; meanwhile, the dosage of acid and the dosage of post-treatment alkali are greatly reduced, and three wastes are reduced, so that the post-treatment is simple, the product is easy to separate, the operation is simple and convenient, side reactions are few, the yield is high, the product purity is high and the process pollution is small.

Description

technical field [0001] The invention relates to a preparation method of m-nitrobenzotrifluoride, which belongs to the technical field of organic synthesis. Background technique [0002] m-Nitrotrifluorotoluene is an important raw material for the synthesis of widely used herbicides—phenylheteroaryl formic acid and phenylheteroaryl thioformate, etc. important raw material. m-Nitrobenzotrifluorotoluene products are mainly supplied to the global market. [0003] At present, the method for preparing m-nitrobenzotrifluoride is to use trifluorotoluene as raw material, and obtain the product through mixed acid nitration of sulfuric acid and nitric acid. However, the method has harsh reaction conditions and high risk. This is mainly due to the fact that the reaction is carried out under mixed acid conditions, and temperature control is difficult. Specifically, the nitration reaction is an exothermic reaction, and the higher the temperature, the faster the nitration reaction speed....

Claims

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Application Information

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IPC IPC(8): C07C205/11C07C201/08
CPCC07C201/08C07C205/11
Inventor 宫宁瑞
Owner BEIJING GREENCHEM TECH
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