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Preparation method for bromopentafluorobenzene

A technology of pentafluorobromobenzene and pentafluorobenzoic acid is applied in the synthesis field of pentafluorobromobenzene, and can solve the problems of harsh bromination conditions, low pentafluorobromobenzene yield and high cost of raw materials

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is a method to synthesize pentafluorobromobenzene with hexafluorobenzene as a raw material, but the raw material cost is too high; using pentafluorobenzene as raw material and liquid bromine to synthesize pentafluorobromobenzene through bromination reaction, the bromination conditions are very harsh; pentafluorobenzene and N The yield of pentafluorobromobenzene synthesized from -bromosuccinimide (NBS) without catalyst is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Weigh 0.1mol of pentafluorobenzoic acid solid and add it to a three-necked flask containing 0.5mol N, N-dimethylaniline, rapidly heat up to a temperature of 70-75 degrees Celsius, and collect the product pentafluorobenzene through a condenser tube and a receiving bottle. After purification, it can be used for bromination reaction.

Embodiment 2

[0012] Add a certain amount of sulfuric acid with a concentration of 50% to 70% in the three-necked flask, add 0.1mol pentafluorobenzene under stirring, control the temperature of 30 degrees Celsius, and add 16.7g of potassium bromate in batches, and the process takes about 30 minutes. After the addition, continue to stir and react at 50 degrees Celsius for 1.5 to 2.5 hours, pour the reaction solution into a mixture of ice and water, extract with carbon tetrachloride, and wash the organic phase with 5% NaHSO3, 10% NaHCO3 solution and distilled water respectively. Dry over sodium sulfate, distill carbon tetrachloride under normal pressure, take a sample for GC analysis, and obtain fluorine-free bromobenzene with a yield of about 34%.

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Abstract

The invention provides a preparation method for bromopentafluorobenzene. The bromopentafluorobenzene is prepared by undergoing decarboxylation and bromination two-step reactions on phenyl-pentafluoride. The reaction operation is simple and practicable, and the method has industrial production application value.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a synthesis method of pentafluorobromobenzene. Background technique [0002] 2,3,4,5,6-pentafluorobromobenzene is an important new type of fine chemical intermediate, it is not only a pharmaceutical intermediate, a pesticide intermediate and a liquid crystal material intermediate, but also an intermediate of olefin polymerization catalysts. application and development prospects. At present, there are many synthesis methods of pentafluorobromobenzene, but there are a series of disadvantages. There is a method to synthesize pentafluorobromobenzene with hexafluorobenzene as a raw material, but the raw material cost is too high; using pentafluorobenzene as raw material and liquid bromine to synthesize pentafluorobromobenzene through bromination reaction, the bromination conditions are very harsh; pentafluorobenzene and N The yield of pentafluorobromobenzene synthesized fro...

Claims

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Application Information

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IPC IPC(8): C07C25/13C07C17/00
Inventor 柳叶张巍
Owner SHANGHAI SINOFLUORO SCI
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