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A kind of preparation method of hydroxy ketone photoinitiator intermediate aryl alkyl ketone

A technology for the synthesis of aryl alkyl ketones and aryl alkyl ketones, which is applied in the field of preparation of (substituted) phenyl alkyl ketones, and can solve problems such as poor reaction selectivity, high reaction temperature, and unsatisfactory reaction yields

Active Publication Date: 2020-10-27
湖南久日新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some problems, such as unsatisfactory reaction yield (US3660491), high reaction temperature (US4950763), complex catalyst preparation process (US2007100166), poor reaction selectivity (WO2002006198), etc., still need to be optimized to be suitable for industrialization

Method used

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  • A kind of preparation method of hydroxy ketone photoinitiator intermediate aryl alkyl ketone
  • A kind of preparation method of hydroxy ketone photoinitiator intermediate aryl alkyl ketone
  • A kind of preparation method of hydroxy ketone photoinitiator intermediate aryl alkyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Preparation of isobutyrylbenzene

[0037] In a nitrogen atmosphere, take 108.1g (0.75mol) of sodium benzoate, 55.0g (0.50mol) of sodium isobutyrate, 11.6g (0.05mol, particle size less than 50nm) of ferroferric oxide, and 200mL of lead oil, and stir well. After 2 hours of reaction, the reflux device is changed to a distillation device to slowly distill the products and low boilers. After 16 hours, when almost no product is evaporated at this temperature, the temperature is reduced to room temperature. The obtained distillate was 65.9 g of colorless or light yellow oil. The distillate was detected to contain 93.2% isobutyrylbenzene by GC, and further purified by vacuum distillation to obtain 59.3g of isobutyrylbenzene colorless liquid with a purity of more than 99%.

Embodiment 2

[0038] Example 2: Preparation of cyclohexyl benzophenone

[0039] In a nitrogen atmosphere, take 144.1g (1.0mol) of sodium benzoate, 75.1g (0.50mol) of sodium cyclohexanoate, 17.4g (0.075mol, particle size less than 50nm) of ferroferric oxide, and reducer oil (boiling point is 350-410) ℃) 250mL, after stirring evenly, the temperature is raised to about 280℃, after 2 hours of reaction, the reflux device is changed to a distillation device, and the products and low boilers are slowly distilled out. After 20h, there is almost no product steaming at this temperature. When the product was discharged, the temperature was lowered to room temperature to obtain 77.2g of a colorless or light yellow oil. The distillate was determined to contain 90.2% cyclohexyl benzophenone by GC, and then further purified by vacuum distillation to obtain a colorless cyclohexyl benzophenone. Liquid 66.4g, purity over 99%.

Embodiment 3

[0040] Example 3: Preparation of cyclohexyl benzophenone

[0041] In a nitrogen atmosphere, take 144.1g (1.0mol) of sodium benzoate, 75.1g (0.50mol) of sodium cyclohexanoate, 17.4g (0.075mol, particle size less than 100nm) of ferroferric oxide, and reduced line oil (boiling point of 350-410) ℃) 250mL, after stirring evenly, the temperature is raised to about 280℃, after 2 hours of reaction, the reflux device is changed to a distillation device, and the products and low boilers are slowly distilled out. After 20h, there is almost no product steaming at this temperature. When it was discharged, the temperature was lowered to room temperature to obtain 66.2 g of a colorless or light yellow oil. The distillate was determined to contain 90.2% of cyclohexyl benzophenone by GC, and then further purified by vacuum distillation to obtain a colorless cyclohexyl benzophenone. The liquid is 60.4g, and the purity is over 99%.

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Abstract

The invention relates to a method for preparing an intermediate aryl alkyl ketone of a hydroxy-ketone photoinitiator and particularly relates to a method for preparing (substituted) phenyl alkyl ketone. According to the method, the product is separated during reaction, the process is simple, and the production cycle is shortened; a catalyst and a solvent are easily and circularly applied mechanically; the product yield is high, and the production cost is low; and the entire reaction process is environmentally friendly.

Description

Technical field [0001] The content of the present invention relates to a preparation method of hydroxy ketone photoinitiator intermediate aryl alkyl ketone, in particular to a preparation method of (substituted) phenyl alkyl ketone. Background technique [0002] α-Hydroxyaromatic ketone photoinitiators are a class of compounds with derivation potential due to their dual active functional groups. Various compounds such as vicinal diols and o-diketenone can be derived, which are widely used in many fields such as UV-curing medicines, pesticides, perfumes, etc . Typical representatives are photoinitiators 1173, 184, 2959, etc. They are not only suitable for general photopolymerization systems, but also for emulsion or latex photopolymerization systems and water-soluble photopolymerization systems, so they are widely used in electronic optical fiber printing and packaging, Adhesives, coating wood, metal, plastics and composite materials. The key intermediate for the preparation of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/48C07C45/82C07C49/76C07C49/792C07C49/807
CPCC07C45/48C07C45/82C07C49/76C07C49/792C07C49/807Y02P20/584
Inventor 张建锋武瑞张齐杨天艳罗想毛桂红
Owner 湖南久日新材料有限公司
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