Synthesis method of 2,4-dichloro-5-fluorin(trichloromethyl)benzene

A technology of trichloromethyl and synthetic methods, applied in the field of chemical technology, can solve the problem of many reaction by-products, achieve the effects of convenient recycling, lower reaction temperature, and higher reaction efficiency

Active Publication Date: 2018-09-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The process adopts chlorination reaction to prepare the trichloride of corresponding toluene, the process is simple, but there are many reaction by-products

Method used

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  • Synthesis method of 2,4-dichloro-5-fluorin(trichloromethyl)benzene
  • Synthesis method of 2,4-dichloro-5-fluorin(trichloromethyl)benzene
  • Synthesis method of 2,4-dichloro-5-fluorin(trichloromethyl)benzene

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Experimental program
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Effect test

Embodiment 1-1

[0024] 35.2 g of bis(1-ethyl-3-methylimidazolium chloride) and 52.3 g of AlCl 3 Place in a nitrogen-protected reaction vessel and stir at normal temperature to obtain 87.5g of 1,2-bis(N-methylimidazolium)ethane chloroaluminate ([C 2 mim][Cl 2 ]-AlCl 3 ).

Embodiment 2-1

[0027] Add 16.5 g (0.1 mol) of 2,4-dichlorofluorobenzene, CCl 4 75g (0.4mol), ionic liquid [C 2 mim][Cl 2 ]-AlCl 3 87.5g, heat up to 60°C and keep warm for 4 hours; after the reaction, let stand to separate and separate, recover the upper ionic liquid, and the lower organic phase is distilled under reduced pressure to obtain the target product 2,4-dichloro-5-fluoro-(trichloro Methyl)benzene 24.2g, Mp: 293~294°C, yield 92.9%.

Embodiment 2-2

[0029] Add 16.5 g (0.1 mol) of 2,4-dichlorofluorobenzene, CCl 4 75g (0.4mol), the ionic liquid [C that embodiment 2-1 reclaims 2 mim][Cl 2 ]-AlCl 3 87.5g, heat up to 60°C and keep warm for 3 hours; after the reaction is over, let it stand for stratification, recover the upper ionic liquid, and the lower organic phase is distilled under reduced pressure to obtain the target product 2,4-dichloro-5-fluoro-(trichloro Methyl)benzene 23.3g, Mp: 293~294°C, yield 92.5%.

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Abstract

The invention belongs to the field of chemical technologies, and particularly relates to a synthesis method of 2,4-dichloro-5-fluorin(trichloromethyl)benzene. According to the method, 2,4-dichlor fluorbenzene and CCl4 are used as starting materials, under the action of ionic liquid 1,2-bis(N-methylimidazolium)ethane chlorine aluminate([C2mim][Cl2]-AlCl3), the 2,4-dichloro-5-fluorin(trichloromethyl)benzene is generated through reaction. The method has the advantages that the ionic liquid catalyst [C2mim][Cl2]-AlCl3) can be conveniently recovered and reused, the yield is high, and the proportionof a bipolymer by-product is reduced; by means of the method, the problem of using lots of alchlor as trichlorine methylation is solved, by using the ionic liquid, the usage amount of the CCl4 is reduced, and meanwhile, due to no post-reaction treatment, lots of acid water is avoided.

Description

technical field [0001] The invention belongs to the field of chemical technology, and in particular relates to a synthesis method of 2,4-dichloro-5-fluoro(trichloromethyl)benzene. Background technique [0002] 2,4-dichloro-5-fluoro(trichloromethyl)benzene is a class of important organic intermediates with a wide range of uses, mainly for the synthesis of 2,4-dichloro-5-fluorobenzoyl chloride, and then Widely used in medicine, pesticides, dyes and other fields. [0003] The methods of 2,4-dichloro-5-fluoro(trichloromethyl)benzene reported in the literature mainly include: [0004] 1) With 2,4-dichloro-5-fluoro-1-methylbenzene as the starting material, 2,4-dichloro-5-fluoro(trichloromethyl)benzene is generated by chlorination reaction, the reaction formula is as follows : [0005] [0006] The process adopts chlorination reaction to prepare corresponding trichloride of toluene, and the process is simple, but there are many reaction by-products. [0007] 2) With 2,4-dich...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/269C07C25/13
CPCC07C17/269C07C25/13
Inventor 吕新宇邱滔汪文丞
Owner CHANGZHOU UNIV
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