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Method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'

A technology of trimethylbenzoyl and diphenylphosphine oxide, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., and can solve the problem of total yield decline and post-processing steps Many problems, to achieve the effect of low cost, simple operation, and meet market demand

Active Publication Date: 2017-10-31
INSIGHT HIGH TECH JIANGSU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the preparation process of diphenylphosphine oxide, there are many post-treatment steps, and a large amount of triethylamine hydrochloride needs to be processed. After the triethylamine hydrochloride is separated, distillation treatment is required to separate diphenylethoxyphosphine out, resulting in a decrease in the overall yield of the two-step reaction

Method used

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  • Method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In a 100ml reaction flask, add 25g of toluene and 3.45g of metal sodium particles (0.15mol), stir, then add 6.9g of ethanol (0.15mol) dropwise, and keep the temperature at 50-55°C during the dropwise addition. After the dropwise addition, stir for 2 hours, add 29.8 g (0.135 mol) of diphenylphosphine chloride dropwise to the reaction system, control the temperature at -10 to 0°C, after the dropwise addition, stir for 1 hour, continue to drop 2, 24.6g (0.135mol) of 4,6-trimethylbenzoyl chloride, the temperature was controlled at 70-75°C during the dropwise addition, and then stirred for 5h.

[0023] After the reaction was completed, 15 g of water was added to the reaction mass, stirred for 1 h, and allowed to stand for stratification. The obtained organic phase was adjusted to a pH value of 7 to 8 with saturated aqueous sodium bicarbonate solution, and the aqueous phase was separated, and the organic phase was washed and layered with water to obtain the organic phase. Pha...

Embodiment 2

[0025] In a 100ml reaction bottle, add 30g of xylene and 3.45g of metal sodium particles (0.15mol), stir, and add 6.9g (0.15mol) of ethanol dropwise, keeping the temperature at 55-60°C during the dropwise addition. After the dropwise addition, stir for 2h, add 30.9g (0.14mol) of diphenylphosphine chloride dropwise to the reaction system, control the temperature at -5~5°C, after the dropwise addition, stir for 1h, continue to dropwise add 2, 27.4g (0.15mol) of 4,6-trimethylbenzoyl chloride, the temperature was controlled at 75-80°C during the dropwise addition, and stirred for another 5h.

[0026] After the reaction was completed, 15 g of water was added to the reaction mass, stirred for 1 h, and allowed to stand for stratification. The obtained organic phase was adjusted to a pH value of 7 to 8 with saturated aqueous sodium bicarbonate solution, and the aqueous phase was separated, and the organic phase was washed and layered with water to obtain the organic phase. Phase dehyd...

Embodiment 3

[0028] In a 100ml reaction flask, add 32g of toluene and 3.45g of metal sodium particles (0.15mol), stir, and add 6.9g of ethanol (0.15mol) dropwise, keeping the temperature at 65-70°C during the dropwise addition. After the dropwise addition, stir for 2h, add 33.1g (0.15mol) of diphenylphosphine chloride dropwise to the reaction system, control the temperature at 5-10°C, after the dropwise addition, stir for 1h, continue to dropwise add 2,4 , 30.1g (0.16mol) of 6-trimethylbenzoyl chloride, the temperature was controlled at 70-75°C during the dropwise addition, and stirred for another 5h.

[0029] After the reaction was completed, 15 g of water was added to the reaction mass, stirred for 1 h, and allowed to stand for stratification. The obtained organic phase was adjusted to a pH value of 7 to 8 with saturated aqueous sodium bicarbonate solution, and the aqueous phase was separated, and the organic phase was washed and layered with water to obtain the organic phase. Phase dehy...

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Abstract

The invention aims to provide a method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'. According to the preparation method, a sodium, ethanol, chlorodiphenylphosphine and 2,4,6-trifluoromethyl benzoyl chloride 'one-pot process' is firstly adopted for replacing the original diphenyl oxethyl phosphine and acyl chloride process for preparing 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, so that the method can greatly reduce the preparation steps and processes, has the characteristics of low cost, simplicity in operation and high yield and can more effectively meet the increasing market requirements at present.

Description

technical field [0001] The invention relates to a synthesis process of a photoinitiator, in particular to a "one-pot" synthesis method of the photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO). Background technique [0002] 2,4,6-Trimethylbenzoyl-diphenylphosphine oxide (TPO) is a highly efficient free radical photoinitiator, which is widely used due to its large absorption in the ultraviolet and visible light regions. It is used in the field of curing of colored systems and film thickness. [0003] Regarding the synthesis of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), there are currently two main synthetic methods in the industry, one is the oxidation process after the addition of aldehydes and halogenated phosphorus, The other is the process of diphenylethoxyphosphine and acid chloride. Chinese patent CN103333206 A discloses the latter method, using diphenylphosphine chloride as a starting material, preparing diphenylethoxyphosphine by reacting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5337
Inventor 胡圣祥朱江任杰张杰张红松施海斌张洪秦辉袁忠华李冬梅吴国平孙贤
Owner INSIGHT HIGH TECH JIANGSU CO LTD
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