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Preparation method of (3, 5-difluorophenyl) diphenylphosphine oxide

A technology of diphenylphosphine oxide and difluorophenyl is applied in the field of preparation of diphenylphosphine oxide, which can solve the problems of single structure and few types of polymers, and achieves high safety, easy modification and excellent oxidation resistance. Effect

Inactive Publication Date: 2020-12-25
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the types of polymers covered by this prior art are relatively small, and the structure is relatively simple.

Method used

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  • Preparation method of (3, 5-difluorophenyl) diphenylphosphine oxide
  • Preparation method of (3, 5-difluorophenyl) diphenylphosphine oxide
  • Preparation method of (3, 5-difluorophenyl) diphenylphosphine oxide

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preparation example Construction

[0020] A preparation method of (3,5-difluorophenyl) diphenylphosphine oxide, comprising:

[0021]

[0022] The preparation method comprises: adding 1-bromo-3,5-difluorobenzene solution into a reaction solvent containing magnesium powder, and performing a Grignard reaction at 0° C. to room temperature for 2-6 hours in a nitrogen or argon atmosphere to obtain 3,5-difluorophenylmagnesium(II) bromide; then mix 3,5-difluorophenylmagnesium(II) bromide with diphenylphosphine chloride solution and react at 0°C to room temperature for 8 -16h, after quenching the reaction with 0.5-1.5mol / L dilute sulfuric acid, dilute hydrochloric acid or dilute phosphoric acid, the light brown oily product is obtained through the first purification treatment; finally, the light brown oily product is treated with hydrogen peroxide or tert-butyl hydroperoxide Oxidation, and after the second purification treatment, (3,5-difluorophenyl) diphenylphosphine oxide is obtained.

[0023] Wherein, the 1-bromo...

Embodiment

[0026] A preparation method of (3,5-difluorophenyl) diphenylphosphine oxide, comprising:

[0027]

[0028] 1) In a 250mL round-bottomed flask equipped with a stirring bar, an addition funnel, a condenser and a gas inlet, continuously feed nitrogen gas, and add 1.2715g of Mg scraps and 20mL of tetrahydrofuran to fully immerse the Mg scraps in tetrahydrofuran, and then add 100mL of Containing 10.6743g of 1-bromo-3,5-difluorobenzene in tetrahydrofuran solution, and continuously stirring at room temperature for 4h to obtain 3,5-difluorophenylmagnesium bromide solution;

[0029] 2) Add 3,5-difluorophenylmagnesium bromide solution dropwise to 50mL tetrahydrofuran solution containing 11.2953g diphenylphosphine chloride through the addition funnel at 0°C, and the resulting reaction mixture was stirred overnight (12h) , was added to 100mL 1M hydrochloric acid to quench;

[0030] 3) Dilute the obtained reaction product mixture with 300mL ethyl acetate, and transfer to a separatory f...

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Abstract

The invention relates to (3, 5-difluorophenyl) diphenylphosphine oxide and a preparation method thereof, the structural formula of the (3, 5-difluorophenyl) diphenylphosphine oxide is shown in the specification, and the preparation method comprises the following steps: firstly, under the protection of inert gas, mixing a solution containing 1-bromine- 3, 5-difluorobenzene and a reaction solution containing Mg powder, and carrying out Grignard reaction; adding a solution containing diphenyl phosphine chloride, mixing, and reacting at the temperature of 0 DEG C to room temperature; then, after purification treatment, obtaining an oily product; and finally, sequentially carrying out oxidation and purification treatment on the oily product to obtain the (3, 5-difluorophenyl) diphenylphosphineoxide. Compared with the prior art, the preparation method has the advantages of simple operation, no need of heating, easily available raw materials, high safety and the like, and the phosphine oxidegroup of the obtained compound has good water absorption and moisture retention and oxidation resistance stability, and can be applied to the fields of fuel cells, ion exchange resin, membrane separation, sensors and other functional materials.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to a preparation method of (3,5-difluorophenyl)diphenylphosphine oxide. Background technique [0002] Proton exchange membrane fuel cell is a clean and efficient new energy power generation device, which has received extensive attention. Proton exchange membrane is one of the core components of fuel cells. Currently, Nafion membrane produced by DuPont is a widely used commercial membrane. However, the disadvantages of Nafion membrane, such as high price, poor resistance to methanol, and sharp drop in conductivity under high temperature and low humidity environment, limit its further development. Therefore, sulfonated aromatic polymer proton exchange membrane has become a research hotspot at present. Among them, the selection of suitable organic monomers has become the primary research direction. The phosphine oxide group contained in the sulfonated polyarylene (thio) ethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53H01M8/1034H01M8/1072C08G65/34C08G75/04
CPCC07F9/5325H01M8/1034H01M8/1072C08G65/34C08G75/04Y02E60/50
Inventor 廖慧英毛松丽鲁晨
Owner SHANGHAI INST OF TECH
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