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Preparation method for boron difluoride diphenyl sulphur tetrafluoroborate compound

A technology of difluorooxyboron diphenylpyrurium tetrafluoroboric acid and compounds, which is applied in the field of preparation of difluorooxyboron diphenylpyrurium tetrafluoroboric acid compounds, can solve problems such as not existing, and achieve simple preparation process and high reaction product High yield and good product stability

Inactive Publication Date: 2016-05-04
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no bibliographic report on the use of diphenyl sulfoxide for initiating polymer polymerization

Method used

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  • Preparation method for boron difluoride diphenyl sulphur tetrafluoroborate compound
  • Preparation method for boron difluoride diphenyl sulphur tetrafluoroborate compound
  • Preparation method for boron difluoride diphenyl sulphur tetrafluoroborate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 5ml of toluene and 0.0005mol of diphenyl sulfoxide to a three-necked flask equipped with a stirring bar to dissolve them, and then add 0.001mol of BF 3 Diethyl ether solution, keep the solution temperature not exceeding 20°C, stir for 20 minutes, add 20ml of n-heptane to precipitate, and separate the liquid with a separatory funnel to obtain a brown liquid in the lower layer, with a yield of 95%.

[0021] figure 1 Infrared image of the target product.

Embodiment 2

[0023] Add 5ml of benzene and 0.0005mol of diphenyl sulfoxide to a three-necked flask equipped with a stirring bar to dissolve them, and then add 0.001mol of BF 3 Diethyl ether solution, keep the solution temperature at 25° C., stir for 15 minutes, add 15 ml of n-heptane to precipitate, and separate the liquid with a separatory funnel to obtain a brown liquid in the lower layer, with a yield of 93%.

Embodiment 3

[0025] Add 5ml of toluene and 0.0005mol of diphenyl sulfoxide to a three-necked flask equipped with a stirring bar to dissolve them, and then add 0.001mol of BF 3 Diethyl ether solution, keep the solution temperature at 15° C., stir for 30 minutes, add 25 ml of n-hexane to precipitate, and separate the liquid with a separatory funnel to obtain a brown liquid in the lower layer, with a yield of 96%.

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Abstract

The invention relates to a preparation method for a boron difluoride diphenyl sulphur tetrafluoroborate compound. The method includes the steps that diphenyl sulfoxide is dissolved in an organic solvent, boron trifluoride is slowly dripped with stirring, and after dripping is finished, the solution is stirred for 10-50 min to ensure a complete reaction; an excess precipitator is added into the obtained solution, separation is carried out, and the boron difluoride diphenyl sulphur tetrafluoroborate compound is obtained. Compared with the prior art, the method has the advantages that the boron difluoride diphenyl sulphur tetrafluoroborate compound prepared through the method is brown liquid, the preparation process is simple, reaction conditions are mild, reaction time is short, the yield of the reaction product is high, the stability of the product is good, and the product can be applied to ring-opening polymerization of tetrahydrofuran and copolymers thereof.

Description

technical field [0001] The invention relates to a preparation method of difluorooxyboron diphenylpyridine tetrafluoroboric acid compound. Background technique [0002] As a chemical raw material, diphenyl sulfoxide is widely used in the production of intermediates of ionic photoinitiators, for example, intermediates of photoacid generators in photoresists, uranium (VI) extractants, rare earth luminescent materials Ligands and the preparation of certain inorganic salt crystals, etc. However, there is no literature report on using diphenyl sulfoxide to initiate polymer polymerization. Contents of the invention [0003] The invention proposes a method for preparing a reaction product with high yield and good stability of the product, and the preparation method of difluorooxyboron diphenylpyridine tetrafluoroboric acid compound. [0004] The technical scheme adopted by the present invention to solve the above-mentioned technical problems is: a preparation method of difluoroo...

Claims

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Application Information

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IPC IPC(8): C07F5/02C08G65/20
CPCC07F5/022C08G65/20
Inventor 周立民袁旭杨静怡张静李琬孟章鹏
Owner WUHAN INSTITUTE OF TECHNOLOGY
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