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Preparing method of 2,6-difluoro-4-bromophenol

A technology of difluorobromobenzene and bromophenol, which is applied in the field of preparation of 2,6-difluoro-4-bromophenol, can solve the problems of product distillation, high production cost, and high safety risk, and achieve low cost and easy Effects of purchasing and reducing operating costs

Active Publication Date: 2015-11-25
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the shortcomings of the traditional 2,6-difluoro-4-bromophenol synthesis method, such as high safety risk, high production cost, and product distillation, etc., and provide a 2,6-difluoro-4-bromophenol that is safe and low in production cost. The preparation method of 6-difluoro-4-bromophenol

Method used

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  • Preparing method of 2,6-difluoro-4-bromophenol
  • Preparing method of 2,6-difluoro-4-bromophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Under the protection of nitrogen, add 60.6g of diisopropylamine and 127g of methyl tert-butyl ether into a clean and dry three-necked flask, stir mechanically and lower the temperature to -55°C, and add 240ml of normal The n-hexane solution of butyllithium (the molar concentration of n-butyllithium is 2.5 mol / L), was kept at -55~-50°C for 0.5 hours after dropping, and the LDA reagent was obtained after the keeping.

[0025] 2) Under nitrogen protection, add 115.8g (0.6mol) of 3,5-difluorobromobenzene and 150g of methyl tert-butyl ether into a clean and dry three-necked flask, start stirring, and cool down to the inner temperature of -55°C. Add the LDA reagent obtained in 1) dropwise at an internal temperature of -55~-50°C, and keep warm at -55~-50°C for 2 hours after the dropwise addition;

[0026] 3) After the heat preservation is over, control the internal temperature of the system obtained in 2) to be -55~-50°C, add 81.2g (0.78mol) of trimethyl borate dropwise to ...

Embodiment 2

[0031] 1) Under the protection of nitrogen, add 60.6g of diisopropylamine and 120g of methyl tert-butyl ether into a clean and dry three-necked flask, stir mechanically and lower the temperature to -55°C, and add 240ml of secondary The n-hexane solution of butyllithium (the molar concentration of sec-butyllithium is 2.5 mol / L), was kept at -55~-50°C for 0.5 hours after dropping, and the LDA reagent was obtained after the keeping.

[0032] 2) Under nitrogen protection, add 115.8g (0.6mol) of 3,5-difluorobromobenzene and 150g of methyl tert-butyl ether into a clean and dry three-necked flask, start stirring, and cool down to the inner temperature of -55°C. Control the internal temperature at -55~-50°C and add the reaction solution in 1) dropwise, and keep it at -55~-50°C for 2 hours after dropping,

[0033] 3) After the heat preservation is completed, control the internal temperature of the system obtained in 2) to be -55~-50°C, add 146.6g (0.78mol) triisopropyl borate dropwise,...

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Abstract

The invention relates to a preparing method of 2,6-difluoro-4-bromophenol, in the preparing method, 1-bromo-3,5-difluorobenzene is taken as a raw material, and high purity 2,6-difluoro-4-bromophenol can be prepared by metallization reaction and oxidation reaction. According to a synthesis route of the preparing method, a raw material of low price is adopted, the product is low in cost, easy to operate, and suitable for large-scale and continuous production, and has a very high application prospect.

Description

technical field [0001] The invention relates to a preparation method of 2,6-difluoro-4-bromophenol, which belongs to the field of chemical synthesis. Background technique [0002] 2,6-Difluoro-4-bromophenol is an important intermediate for the synthesis of various liquid crystal monomers. On the one hand, it can undergo etherification reactions with halogen-containing benzene rings, and on the other hand, it can also perform etherification reactions with various boric acids. The coupling reaction prepares fluorine-containing liquid crystal monomers with different properties. This type of liquid crystal monomer has the advantages of low viscosity, high resistivity, fast response speed, and can improve the dielectric constant of mixed crystals. It is very suitable for driving thin film field effect transistors. LCD display. 2,6-difluoro-4-bromophenol, as an important intermediate in the synthesis of various fluorine-containing liquid crystal monomers, has a very good applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/01C07C39/27C07F5/02
CPCC07C37/01C07F5/025C07C39/27
Inventor 王磊李鹏周立平沈清于晓伟乔松游瑞行
Owner VALIANT CO LTD
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