Synthetic method for 2,4-difluorobiphenyl

A technology of difluorobiphenyl and synthesis method, which is applied in the field of synthesis of 2,4-difluorobiphenyl and 2,4-difluorobiphenyl, and can solve the problems of lengthy reaction steps, low yield, complicated operation, etc. To achieve the effect of short process, simple reaction process and avoid high temperature reaction

Active Publication Date: 2018-10-16
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a synthetic method of 2,4-difluorobiphenyl to solve the problems of low yield, complicated operation and lengthy reaction steps of 2,4-difluorobiphenyl

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 114g (1mol) of trifluoroacetic acid (1mol), 5.7g of anhydrous magnesium sulfate, 1.3g of catalyst and 134ml of benzene (1.5mol) into the reaction kettle, stir and cool to 2°C, add 128.9g (1.1mol) of isoamyl nitrite, Control the temperature at 6°C, add 130.1g (1mol) of 2,4-difluoroaniline dropwise therein, control the reaction temperature at 10°C during the dropwise addition process, stir and react at 5°C for 1h after the addition, and put the reaction The mixture was filtered with suction, washed with benzene three times, then washed with water until neutral, dried and distilled under reduced pressure to obtain a light yellow solid.

[0020] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 20 minutes, decarburize and filter, put the filtrate into the crystallization kettle, and when the temperature of the crystallization kettle drops to 10°C, discharge the material for solid-liquid separ...

Embodiment 2

[0023] Add 34.2g (0.3mol) of trifluoroacetic acid, 10.26g of anhydrous magnesium sulfate, 0.52g of catalyst and 35.5ml of benzene (0.4mol) into the reaction kettle, stir and cool to 3°C, add 35.2g (0.3mol) of isoamyl nitrite mol), the temperature was controlled at 7°C, 26.02g (0.2mol) of 2,4-difluoroaniline was added dropwise therein, the reaction temperature was controlled to be 15°C during the dropwise addition, and the reaction was stirred at 7°C for 1.5h after the addition was completed. After the reaction, the reaction mixture was suction filtered, washed with benzene three times, then washed with water until neutral, dried, and distilled under reduced pressure to obtain a light yellow solid.

[0024] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 25 minutes, decarburize and filter, and put the filtrate into the crystallization kettle. When the temperature of the crystallization kettle drops...

Embodiment 3

[0027] Add 68.4g (0.6mol) of trifluoroacetic acid, 13.68g of anhydrous magnesium sulfate, 0.98g of catalyst and 71ml of benzene (0.8mol) into the reaction kettle, stir and cool to 4°C, add 70.4g (0.6mol) of isoamyl nitrite ), control the temperature at 8°C, add 65.05g (0.5mol) of 2,4-difluoroaniline dropwise therein, control the reaction temperature at 17°C during the dropwise addition process, stir and react at 9°C for 2h after the addition, and the reaction ends Afterwards, the reaction mixture was suction filtered, washed with benzene three times, and then washed with water until neutral, dried, and distilled under reduced pressure to obtain a light yellow solid.

[0028] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 30 minutes, decarburize and filter, and put the filtrate into the crystallization kettle. When the temperature of the crystallization kettle drops to 10°C, discharge the material...

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Abstract

The invention discloses a synthetic method for 2,4-difluorobiphenyl, and belongs to the technical field of halogenated biphenyl. The method uses 2,4-difluoroaniline and benzene as raw materials, the 2,4-difluoroaniline is diazotized, and the diazotized product and the benzene are subjected to a coupling reaction to obtain the 2,4-difluorobiphenyl; and the method comprises the following steps: adding trifluoroacetic acid, anhydrous magnesium sulfate, a catalyst and the benzene into a reaction kettle, performing cooling under stirring to temperature of 2-6 DEG C, adding isoamyl nitrite, controlling temperature at 6-10 DEG C, adding the 2,4-difluoroaniline dropwise, controlling reaction temperature at 10-25 DEG C in the adding process, after material addition is completed, performing a reaction under stirring for 1-3 h at temperature of 5-12 DEG C, after the reaction is completed, performing suction filtration on the reaction mixture, performing washing, performing drying, and performingreduced-pressure distillation to obtain the 2,4-difluorobiphenyl. The synthetic method disclosed by the invention is simple, and the synthesized 2,4-difluorobiphenyl has a high yield and high purity.

Description

technical field [0001] The invention belongs to the technical field of halogenated biphenyls, relates to 2,4-difluorobiphenyls, and specifically relates to a synthesis method of 2,4-difluorobiphenyls. The synthesis method of the invention is simple, and the synthesized 2,4-difluorobiphenyls Benzene has high yield and high purity. Background technique [0002] With the development of my country's electronic information industry, the demand for chemical power is increasing, and its performance requirements are getting higher and higher. Lithium-ion batteries are widely used in various electronic devices such as notebook computers, mobile phones, and MP4s because of their advantages such as high working voltage, high energy density, environmental friendliness, stable cycle, and safety. In recent years, the basic research and application development of lithium-ion batteries have become one of the hot spots. Lithium batteries include positive poles, negative poles, electrolytes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/263C07C25/18C07C245/20
CPCC07C17/263C07C245/20C07C25/18
Inventor 葛建民刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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