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m-Bromobenzotrifluoride and its preparation method

A technology of m-bromotrifluorotoluene and bromotrifluorotoluene is applied in the field of organic chemical industry synthesis, can solve the problems of high energy consumption, high production cost, long process route, etc., and achieves the effects of reducing volatility, toxicity, and low price

Active Publication Date: 2018-03-06
JIANGSU ZHONGNENG CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has problems such as high production cost, long process route, high risk, many three wastes, and high energy loss.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of m-bromobenzotrifluoride, comprising the steps of:

[0023] (1) trifluorotoluene and iron-based catalyst are dropped into the reactor, and the iron-based catalyst quality is 0.05% of the trifluorotoluene quality;

[0024] (2) Add mass concentration again and be the sulfuric acid 200ml of 30% hydrobromic acid and 5mol / L;

[0025] (3) Control the temperature under agitation to be 5-15° C., while gradually dripping a mass concentration of 10-20% sodium chlorite solution; to control the generation of isomers or polybrominated compounds together with the iron-based catalyst;

[0026] (4) After feeding, keep warm at 5°C for 1-2h; then heat up to 20°C for 1-2h;

[0027] (5) Stand still and separate phases: the product after the heating reaction is divided into an organic phase and an aqueous phase, and the organic phase will be washed with water successively, washed with aqueous sodium bicarbonate solution with a mass concentration of 5%-10%, and washed...

Embodiment 2

[0033] A preparation method of m-bromobenzotrifluoride, comprising the steps of:

[0034] (1) trifluorotoluene and iron-based catalyst are dropped into the reactor, and the iron-based catalyst quality is 0.5% of the trifluorotoluene quality;

[0035] (2) Add mass concentration again and be the sulfuric acid 200ml of 30% hydrobromic acid and 5mol / L;

[0036] (3) Control the temperature under agitation to be 15° C., and gradually drop in a mass concentration of 10-20% sodium chlorite solution; to control the generation of isomers or polybrominated substances together with the iron-based catalyst

[0037] (4) After feeding, keep warm at 5°C for 1-2h; then heat up to 20°C for 1-2h;

[0038] (5) Stand still and separate phases: the product after the heating reaction is divided into an organic phase and an aqueous phase, and the organic phase will be washed with water successively, washed with aqueous sodium bicarbonate solution with a mass concentration of 5%-10%, and washed with ...

Embodiment 3

[0043] A preparation method of m-bromobenzotrifluoride, comprising the steps of:

[0044] (1) trifluorotoluene and iron-based catalyst are dropped into the reactor, and the iron-based catalyst quality is 0.3% of the trifluorotoluene quality;

[0045] (2) Add mass concentration again and be the sulfuric acid 200ml of 30% hydrobromic acid and 5mol / L;

[0046] (3) It is 10 DEG C to control the temperature under stirring conditions, while gradually dripping a mass concentration of 10-20% sodium chlorite solution; to control the generation of isomers or polybrominated compounds together with the iron-based catalyst;

[0047] (4) After feeding, keep warm at 15°C for 1-2h; then heat up to 25°C for 1-2h;

[0048] (5) Stand still and separate phases: the product after the heating reaction is divided into an organic phase and an aqueous phase, and the organic phase will be washed with water successively, washed with aqueous sodium bicarbonate solution with a mass concentration of 5%-10...

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PUM

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Abstract

The invention discloses a preparation method of 3-bromobenzotrifluoride.The preparation method includes the steps that firstly, trifluorotoluene and a composite catalyst are put into a reactor, wherein the mass of the composite catalyst is 0.05-0.5% that of trifluorotoluene; secondly, hydrobromic acid with the mass concentration of 30% and 200 ml of 5 mol / L sulfuric acid are added; thirdly, the temperature is controlled to be 5-15 DEG C under the stirring condition, and meanwhile a sodium chlorite solution with the mass concentration of 10-20% is dripped; fourthly, heat preservation is carried out in a low-temperature environment after adding is finished, and then a heating reaction is carried out; fifthly, standing and phase splitting are carried out, wherein a product obtained after the heating reaction is split into an organic phase and an aqueous phase, the aqueous phase is subjected to acid washing to be neutral, and then standing is carried out; sixthly, drying is carried out, and a crude product is obtained; seventhly, the crude product is subjected to reduced pressure distillation, and 3-bromobenzotrifluoride is obtained.The invention further discloses 3-bromobenzotrifluoride prepared with the preparation method.According to the preparation method, generation of bromine which is volatile, highly toxic and difficult to dispose is reduced, and the utilization rate of bromine atoms reaches 90% or above.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to m-bromobenzotrifluoride and a preparation method thereof. Background technique [0002] m-Bromotrifluorotoluene is a very important chemical intermediate, mainly used in the production of pesticides, pharmaceuticals and other fields, such as the synthesis of weight-loss drugs fenfluramine and benflurex. [0003] There are two main synthesis methods of m-bromotrifluoromethylbenzene: 1) direct bromination method. The raw materials of the method are trifluorotoluene and bromine, and iron powder is used as a catalyst. The molar ratio of benzotrifluoride to bromine is 1:1.52, the weight of iron powder is 20% of that of benzotrifluoride, and the yield of methyl benzotrifluoride is about 80%. This method has problems such as low production efficiency, high process risk, and high discharge of three wastes (solid waste, liquid waste, and gas waste). 2) Diazotization and replac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/13C07C17/12
CPCC07C17/12C07C25/13
Inventor 李金祥吴朝阳刘红飞陆鑫华
Owner JIANGSU ZHONGNENG CHEM TECH CO LTD
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