Preparation method of 2-hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone

Abstract

The invention relates to a preparation method of 2-hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone, which comprises the following steps: mixing 2-chloro-1-[4-(2-chloroethoxy) phenyl]-2-methyl-1-acetone with alkali liquor, alkali metal iodide and a phase transfer catalyst, and then carrying out microwave reaction to obtain the 2-hydroxy-1-[4-(2-chloroethoxy) phenyl]-2-methyl-1-acetone. The 2-hydroxyl-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone is subjected to a reaction to obtain 2-hydroxyl-1-[4-(2- Alkali metal iodide and a phase transfer catalyst are added in the reaction process, microwave is combined, double hydrolysis of alpha-chlorine and alkyl chloride is achieved, the target photoinitiator is obtained, the alkaline hydrolysis reaction process has the high yield, the yield of 2-hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone can reach 80% or above, and the yield of 2-hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone can reach 80% or above. The purity can reach 99% or above.

Description

technical field [0001] The invention belongs to the field of photoinitiator preparation, and relates to a preparation method of 2-hydroxy-1-[4-(2-hydroxyethoxy)phenyl]-2-methyl-1-propanone. Background technique [0002] 2-Hydroxy-1-[4-(2-hydroxyethoxy)phenyl]-2-methyl-1-propanone is a kind of α-hydroxy ketone photoinitiator, which has high photoinitiation efficiency and thermal Good stability, yellowing resistance, no peculiar smell; [0003] The prior art discloses a preparation method of a water-soluble photoinitiator 2-hydroxyl-1-[4-(2-hydroxyethoxyl)phenyl]-2-methyl-1-propanone, comprising using 2-hydroxyl Ethyl phenyl ether is used as a raw material. First, carry out a hydroxyl protection reaction with acetic acid, perform a Friedel-Crafts acylation reaction after vacuum distillation and purification, and obtain an alkyl-substituted aromatic ketone, and then carry out a bromination reaction in bromine carbon tetrachloride solution, and Alkaline hydrolysis in sodium me...

AI Technical Summary

Problems solved by technology

[0003] The prior art discloses a preparation method of a water-soluble photoinitiator 2-hydroxyl-1-[4-(2-hydroxyethoxyl)phenyl]-2-methyl-1-propanone, comprising using 2-hydroxyl Ethyl phenyl ether is used as a raw material. First, carry out a hydroxyl protection reaction with acetic acid, perform a Friedel-Crafts acylation reaction after vacuum distillation and purification, and obtain an alkyl-substituted aromatic ketone, and then carry out a bromination reaction in bromine carbon tetrachloride solution, and Alkaline hydrolysis in sodium methoxide methanol solution to obtain the above-mentioned photoinitiator (referring to literature: Sun Yong et al., Shandong Chemical Industry, 2003, (3): 5-9); CN102786405A and CN101811951A each disclose a kind of 2-hydroxyl-1- The preparation method of [4-(2-hydroxyethoxy) phenyl]-2-methyl-1-propanone all comprises: carrying out 2-hydroxyethyl phenyl ether acetate and isobutyryl chloride under Lewis acid catalysis Friedel-Crafts acylation reaction, followed by bromination and alkali hydrolysis to obtain the above-mentioned photoinitiator; the above-mentioned preparation process needs to protect and deprotect the hydroxyl group in the reaction raw material, resulting in a large loss of protective agent acetic acid; in addition, the Friedel-Crafts acylation process Among them, due to the presence of ester groups in the raw materials, a large amount of catalyst will be consumed, which will significantly increase the amount of catalyst used. Taking the amount disclosed in CN101811951A as an example, the amount of catalyst used is 2 to 2.2 times that of isobutyryl chloride. The theoretical dosage of chemical reaction is twice as high, resulting in a large loss of catalyst

Images