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Preparation method and application of photoinitiator intermediate

A photoinitiator and intermediate technology, applied in the field of preparation of photoinitiator intermediates, can solve the problems of poor α-chlorination selectivity, complicated recovery operation, and high cost of bromine, so as to improve chlorination selectivity and increase production The effect of reducing the efficiency and reducing the process cost

Pending Publication Date: 2022-04-12
湖南久日新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN101811951A discloses a preparation method of 2-hydroxyl-1-{4-(2-hydroxyethoxy)phenyl}-2-methyl-1-propanone, using 2-phenoxyethyl acetate as raw material, Carry out Friedel-Crafts reaction with isobutyryl chloride with a molar ratio of 1 to 1.2 equivalents under the catalysis of Lewis acid; then carry out bromination reaction under the catalysis of N,N-dimethylformamide or iodine; use phase transfer at room temperature The catalyst catalyzes the hydrolysis of the bromination product; finally, the product is obtained by purification and crystallization. The above-mentioned preparation method adopts the bromination process, which has high bromine cost and complicated recovery operation; while the traditional chlorination process has poor α-chlorination selectivity, and the product low yield problem

Method used

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  • Preparation method and application of photoinitiator intermediate
  • Preparation method and application of photoinitiator intermediate
  • Preparation method and application of photoinitiator intermediate

Examples

Experimental program
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Embodiment 1

[0079] This embodiment provides a kind of preparation method of photoinitiator 2959, specifically comprises:

[0080] (1) Friedel-Crafts reaction:

[0081] 36g (0.2mol) 2-phenoxyethyl acetate is dissolved in 70g chlorobenzene, obtains 2-phenoxyethyl acetate solution, connects tail gas absorption device (absorbent is ice water), at-3 ℃, Add 56g (0.42mol) of anhydrous aluminum trichloride to the above solution, stir for 0.5h; then raise the temperature to 3°C, with stirring, add 21.3g (0.2mol) of isobutyryl chloride dropwise, the dropwise addition is completed in 2h, and keep warm for 6h , cooling the reaction solution to -3°C, adding it to the ice water of the tail gas absorption device for hydrolysis, stirring for 0.5h, standing for stratification, separating the organic phase, washing with water, to obtain a solution of the compound of formula b;

[0082] (2) Chlorination reaction:

[0083] At 0°C, the solution of the compound of formula b obtained by the Friedel-Crafts rea...

Embodiment 2

[0091] The difference between this embodiment and embodiment 1 is only that the sulfuric acid phase obtained in step (2) is used in step (1), and other parameters and conditions are exactly the same as in embodiment 1.

[0092] The photoinitiator 2959 product obtained in this example is a white solid with a purity of 99.0% and a yield of 89.5%.

Embodiment 3

[0094] The difference between this embodiment and Example 1 is only that the sulfuric acid of 70g 50% is replaced by the sulfuric acid of 54g 65% in the step (2), and other parameters and conditions are exactly the same as in Example 1.

[0095] The photoinitiator 2959 product obtained in this example is a white solid with a purity of 99.0% and a yield of 89.8%.

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Abstract

The invention relates to a preparation method and application of a photoinitiator intermediate, and the preparation method comprises the following steps: mixing 2-(4-isobutyrylphenoxy) ethyl acetate and sulfuric acid with the concentration of 30%-85%, introducing chlorine, and carrying out chlorination reaction to generate the photoinitiator intermediate; wherein the sulfuric acid with the specific concentration is added as an auxiliary agent, the electronic state on a benzene ring in the 2-(4-isobutyryl phenoxy) ethyl acetate can be changed, then the chlorination reaction on methyl of the benzene ring and a protecting group acetyl is inhibited, meanwhile, the keto-carbonyl alpha-chlorination reaction rate is increased, the chlorination selectivity is improved, and the yield is increased. Methyl chlorination of acetyl is avoided, and the yield of alpha-chlorination products is increased; compared with a traditional bromination process, the chlorination process adopted by the invention has the advantages of low process cost and simple recovery operation, and compared with the traditional bromination process, the chlorination process has higher selectivity on alpha-chlorination reaction and higher yield of a target intermediate product.

Description

technical field [0001] The invention belongs to the field of photoinitiator preparation, and relates to a preparation method and application of a photoinitiator intermediate. Background technique [0002] Photoinitiator 2959, Chinese name: 2-hydroxy-2-methyl-1-[4-(2-hydroxyethoxy)phenyl]-1-propanone, is a highly efficient non-yellowing ultraviolet photoinitiator , used to initiate UV polymerization of unsaturated prepolymers and monomers. [0003] CN101811951A discloses a preparation method of 2-hydroxyl-1-{4-(2-hydroxyethoxy)phenyl}-2-methyl-1-propanone, using 2-phenoxyethyl acetate as raw material, Carry out Friedel-Crafts reaction with isobutyryl chloride with a molar ratio of 1 to 1.2 equivalents under the catalysis of Lewis acid; then carry out bromination reaction under the catalysis of N,N-dimethylformamide or iodine; use phase transfer at room temperature The catalyst catalyzes the hydrolysis of the bromination product; finally, the product is obtained by purificat...

Claims

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Application Information

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IPC IPC(8): C07C67/287C07C69/635C07C67/29C07C69/16C07C45/64C07C45/65C07C49/84
Inventor 罗想李钰刘川伟周杨胡祖飞
Owner 湖南久日新材料有限公司
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