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Normal-temperature catalyzed synthesis of 2-bromo-5-fluorobenzotrifluoride

A technology of fluorobenzotrifluoride and normal temperature, which is applied in the field of preparation of chemical intermediate 2-bromo-5-fluorobenzotrifluoride, can solve the problems of environmental hazards, expensive catalysts, high equipment requirements, etc., and achieve significant economic benefits and social benefits. Significant benefits and the effect of reducing production costs

Active Publication Date: 2017-11-10
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] At present, the above-mentioned methods at home and abroad have one or more of the following disadvantages: 1. Organic solvents such as liquid paraffin and halogenated aromatic hydrocarbons need to be used as reaction media, which not only cause a certain degree of harm to the surrounding environment and personnel; 2. The catalyst is expensive , high cost; 3, the reaction needs to be carried out under high temperature conditions, high equipment requirements and high energy consumption

Method used

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  • Normal-temperature catalyzed synthesis of 2-bromo-5-fluorobenzotrifluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 1000mL three-necked flask, under normal temperature and pressure conditions, 100g of 100% sulfuric acid, 200g of m-fluorobenzotrifluoride, 4g of ammonium bromide, 2g of bromosuccinimide, and 4g of tetrabutylammonium bromide were successively added under stirring, Add 97.5 g of bromine dropwise. After the addition, control the conditions of normal temperature and pressure, continue the reaction for 5-6 hours, take a sample, and GC detects that the raw material is less than 1%. Terminate the reaction, remove the catalyst by filtration, transfer to a 1000mL separating funnel, stand still for 1h, separate the bottom acid, put the crude product in a 1000mL bottle, add 500g of water under stirring, drop in 5% sodium hydroxide solution to adjust the pH=7, After alkali washing, the solvent was removed, and the fraction at 158-162°C / mmHg was collected by rectification to obtain 278g of the final product, with a yield of 92.3% and a content of 99%.

Embodiment 2

[0031] In a 1000mL three-necked flask, under normal temperature and pressure, add 100% sulfuric acid 180g, m-fluorobenzotrifluoride 200g, ammonium bromide 1g, bromosuccinimide 0.1g, tetrabutylammonium bromide 1g under stirring , add bromine 195g dropwise, after the addition is completed, control the normal temperature and pressure conditions, continue the reaction for 5-6h, take a sample, and GC detects that the raw material is less than 1%. Terminate the reaction, remove the catalyst by filtration, transfer to a 1000mL separating funnel, stand still for 1h, separate the bottom acid, put the crude product in a 1000mL bottle, add 500g of water under stirring, drop in 5% sodium hydroxide solution to adjust the pH=7, After alkali washing, solvent extraction was performed, and the fraction at 158-162° C. / mmHg was collected by rectification to obtain 275 g of the final product, with a yield of 91.2% and a content of 99%.

Embodiment 3

[0033] In a 1000mL three-necked flask, under normal temperature and pressure conditions, 100g of 100% sulfuric acid, 200g of m-fluorobenzotrifluoride, 4.5g of ammonium bromide, 0.5g of bromosuccinimide, and tetrabutylammonium bromide were successively added under stirring. 4.5g, add 97.5g of bromine dropwise, after the addition is completed, control the normal temperature and pressure conditions, continue the reaction for 5-6h, take a sample, and GC detects that the raw material is less than 1%. Terminate the reaction, remove the catalyst by filtration, transfer to a 1000mL separating funnel, stand still for 1h, separate the bottom acid, put the crude product in a 1000mL bottle, add 500g of water under stirring, drop in 5% sodium hydroxide solution to adjust the pH=7, After alkali washing, the solvent was removed, and the fraction at 158-162°C / mmHg was collected by rectification to obtain 276g of the final product, with a yield of 91.5% and a content of 99%.

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Abstract

The invention discloses a method for preparing 2-bromo-5-fluorobenzotrifluoride. In the method, fluorobenzotrifluoride is used as a raw material, bromine is used as a brominating agent, and the 2-bromo-5-fluorobenzotrifluoride is synthesized in the presence of sulfuric acid and a composite catalyst at normal temperature. By means of the method, the yield reaches 90.0% or above, the purity reaches 99.0% or above, the raw materials used in the reaction process are convenient to purchase, the production cost is low, the waste acid obtained in the reaction process can be recycled, the post-treatment is easy, the reaction conditions are mild, and the method has good economic benefits and social benefits.

Description

a technical field [0001] The invention relates to a method for preparing pesticide chemical products, in particular to a method for preparing a chemical intermediate 2-bromo-5-fluorobenzotrifluoride. The method is applicable to the occasion that 2-bromo-5-fluorobenzotrifluoride is obtained by reacting at normal temperature and pressure with m-fluorobenzotrifluoride as raw material, under the conditions of sulfuric acid and bromide catalyst, bromine as bromination agent. Two background technology [0002] 2-Bromo-5-fluorobenzotrifluoride has the molecular formula C 7 h 3 BrF 4 , with a molecular weight of 243. It has a wide range of uses, and can be prepared as an organic reagent, and at the same time, it can also prepare a pharmaceutical intermediate or a pesticide intermediate. [0003] At present, there are three main process routes for the production of this product reported at home and abroad: [0004] 1) m-fluorobenzotrifluoride is nitrated and reduced to obtain 2-...

Claims

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Application Information

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IPC IPC(8): C07C17/12C07C25/13
CPCC07C17/12C07C25/13
Inventor 韩刘李佳琪刘文宇李琴玉苏杨黄雄郁闯孙世新方东
Owner YANCHENG TEACHERS UNIV
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