Preparation method of 2,4,6-trimethyl benzoyl phenyl ethyl phosphinate

A technology of ethyl trimethylbenzoylphenylphosphinate, which is applied in the field of preparation of ethyl 2,4,6-trimethylbenzoylphenylphosphinate to achieve guaranteed yield and operation simple effect

Active Publication Date: 2014-08-13
CHANGZHOU JIURI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process can overcome the problems of the existing methods, and is a p...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Preparation of ethyl 2,4,6-trimethylbenzoylphenyl phosphinate

[0024] Mix 537g of chlorobenzene and 92.1g of absolute ethanol, cool to 0°C, slowly add 179.0g of phenylphosphine dichloride under stirring, raise to room temperature, monitor the reaction by liquid chromatography, and the reaction is completed in 2.5 hours. Cool to 5°C, slowly add 202g of triethylamine, stir for 1 hour, add 222.3g of 2,4,6-trimethylbenzaldehyde dropwise, raise to room temperature, monitor the reaction by liquid chromatography, after the reaction is completed. Cool to 0°C, maintain the temperature around 0°C, add 14.9g WO 3 , slowly drip the hydrogen peroxide of 226.7g 30%, insulation reaction, liquid chromatography monitors reaction.

[0025] After the reaction was finished, the resulting reaction solution was washed with saturated brine, allowed to stand for layers, and 10% Na was added to the organic phase. 2 SO 3 solution, stirred for 0.5h, and then adjusted to about p...

Embodiment 2

[0027] Example 2: Preparation of ethyl 2,4,6-trimethylbenzoylphenyl phosphinate

[0028] Mix 537g of chlorobenzene and 92.1g of absolute ethanol, cool to 0°C, slowly add 179.0g of phenylphosphine dichloride under stirring, raise to room temperature, monitor the reaction by liquid chromatography, and the reaction is completed in 2.5 hours. Cool to 5°C, slowly add 202g of triethylamine, stir for 1 hour, add 222.3g of 2,4,6-trimethylbenzaldehyde dropwise, raise to room temperature, monitor the reaction by liquid chromatography, after the reaction is over. Cool to 0°C, maintain the temperature around 0°C, add 14.9g WO in turn 3 , slowly drip 257.3g 70% tert-butanol peroxide, keep warm and react, and monitor the reaction by liquid chromatography.

[0029] After the reaction was finished, the resulting reaction solution was washed with saturated brine, allowed to stand for layers, and 10% Na was added to the organic phase. 2 SO 3 solution, stirred for 0.5h, and then adjusted ...

Embodiment 3

[0030] Example 3: Preparation of ethyl 2,4,6-trimethylbenzoylphenyl phosphinate

[0031] Mix 537g of chlorobenzene and 92.1g of absolute ethanol, cool to 0°C, slowly add 179.0g of phenylphosphine dichloride under stirring, raise to room temperature, monitor the reaction by liquid chromatography, and the reaction is completed in 2.5 hours. Cool to 5°C, slowly add 108.0 g of sodium methoxide, stir for 1 h, then dropwise add 222.3 g of 2,4,6-trimethylbenzaldehyde, rise to room temperature, and monitor the reaction by liquid chromatography, after the reaction is complete. Cool to 0°C, maintain the temperature around 0°C, add 14.9g WO in turn 3 , slowly drip the hydrogen peroxide of 226.7g 30%, insulation reaction, liquid chromatography monitors reaction.

[0032] After the reaction was finished, the resulting reaction solution was washed with saturated brine, allowed to stand for layers, and 10% Na was added to the organic phase. 2 SO 3The solution was stirred for 0.5h, and...

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PUM

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Abstract

The invention relates to a preparation method of 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate, and in particular relates to a method for preparing 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate through the steps of carrying out substitution condensation reaction on dichlorophenyl phosphine and ethanol to obtain an intermediate; performing condensation reaction on the intermediate and 2,4,6-trimethyl benzaldehyde under an alkaline condition, and finally performing oxidation by using an oxidant under catalysis of a catalyst. The preparation process of 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate, disclosed by the invention, has the advantages as follows: the influences of an acidic medium on the intermediate can be avoided; the requirements of the condensation reaction between 2,4,6-trimethyl benzaldehyde and phenyl ethyl hypophosphite for reaction equipment can be reduced; meanwhile, the reaction yield can be ensured; the preparation process is simple in operation and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of ethyl 2,4,6-trimethylbenzoylphenyl phosphinate. It specifically relates to an esterification rearrangement reaction with phenylphosphine dichloride and ethanol, and then carries out an addition reaction with 2,4,6-trimethylbenzaldehyde under alkaline conditions, and finally, under the catalysis of a catalyst, is used The oxidant is oxidized to prepare ethyl 2,4,6-trimethylbenzoylphenylphosphinate. Background technique [0002] Ethyl 2,4,6-Trimethylbenzoylphenylphosphinate is a liquid UV photoinitiator for acrylic-based resins and styrene-containing unsaturated polyesters, easy to add to all formulations. Ethyl 2,4,6-trimethylbenzoylphenylphosphinate is widely used as photoinitiator or photosensitizer in various paints, inks and coatings with low extractability, low migration and low volatility . Ethyl 2,4,6-trimethylbenzoylphenylphosphinate absorbs long wavelengths in the UV spectrum, it can also comp...

Claims

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Application Information

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IPC IPC(8): C07F9/32
Inventor 吕振波毛桂红杨天艳石智铭刘川伟罗想武瑞张齐赵国锋
Owner CHANGZHOU JIURI CHEM CO LTD
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