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Preparation method of aryl phenolic ketone

The technology of aryl phenol ketone and alkyl phenol is applied in the field of preparation of aryl phenol ketone, which can solve the problems of complex process and unfriendly environment, and achieve the effects of simplified process route, environmental friendliness and mild reaction conditions.

Pending Publication Date: 2021-05-04
平顶山德源精细化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of aryl phenol ketones, to solve the problems of complex technology and unfriendly environment in the existing methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The arylphenol ketone of the present embodiment is 2-hydroxyl-5-nonylacetophenone, and the preparation method comprises the following steps:

[0019] (1) Add 11g of 4-nonylphenol, 110g of a mixture of acetic acid and acetic anhydride (the mass ratio of the two is 7:3), and 13.6g of zinc dichloride to a 100mL four-necked flask, and heat up to 100 °C, reflux for 10 hours, use TCL to detect the complete reaction of 4-nonylphenol, then stop stirring and cool down to room temperature;

[0020] (2) Steam excess acetic acid and acetic anhydride to obtain a viscous liquid; then mix the viscous liquid with sherwood oil and water, let it stand, and separate the water phase; to obtain an organic phase, mix the primary organic phase with sherwood oil Mix with water, stand still, separate the water phase to obtain the secondary organic phase; carry out normal pressure distillation on the secondary organic phase, distill off the solvent, then carry out vacuum distillation, collect 5m...

Embodiment 2

[0023] The arylphenol ketone of this example is 2-hydroxy-5-nonylacetophenone, and the preparation method refers to the preparation method in Example 1, the only difference is that the reaction temperature in step (1) is 60°C, and the rest are the same . After calculation, the yield of 2-hydroxy-5-nonylacetophenone is 70%, and the purity is 93%.

Embodiment 3

[0025] The arylphenol ketone of this example is 2-hydroxy-5-nonylacetophenone, the preparation method refers to the preparation method in Example 1, the only difference is that the reaction temperature in step (1) is 140°C, and the rest are the same . After calculation, the yield of 2-hydroxy-5-nonylacetophenone was 78%, and the purity was 94%.

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PUM

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of aryl phenolic ketone. The preparation method of the aryl phenolic ketone comprises the following steps: 4-alkylphenol is reacted with an acylating agent under the action of Lewis acid; the reaction temperature is 60 to 160 DEG C; the acylating agent is a mixture of fatty acid and corresponding anhydride, and the mass ratio of the fatty acid to the corresponding anhydride is (5: 5)-(8: 2); wherein the structural formula of the 4-alkylphenol is shown in the specification, the structural formula of the fatty acid is R2-COOH, the structural formula of the aryl phenolic ketone is shown in the specification, R1 is an alkyl group with the number of carbon atoms is 1-12, and R2 is an alkyl group with the number of carbon atoms is 1-19. The aryl phenolic ketone synthesized by the preparation method provided by the invention has high yield, no toxic by-product is generated in the reaction process, and the operation safety is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of aryl phenolic ketones. Background technique [0002] Arylphenol ketone is a raw material for the preparation of ketoxime extractants. Its synthesis method is generally obtained by acylation and rearrangement of alkylphenol under the action of Lewis acid. Commonly used acylating agents are acid chlorides. For example, Yu Linhua et al. used 4-tertoctylphenol to perform esterification reaction with acetyl chloride at 80°C, and then added aluminum chloride to perform Fries rearrangement at 120°C. Obtained 2-hydroxy-5-tert-octyl acetophenone ("Synthesis of 2-hydroxy-5-tert-octyl acetophenone oxime", Hydrometallurgy, August 2014, Vol.33No.4, 292-296 ). The method sequentially synthesizes 2-hydroxy-5-tertoctylacetophenone through esterification and rearrangement in two steps, and uses toxic and corrosive acetyl chloride as an acylating ag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/54C07C49/825
CPCC07C45/54C07C49/825
Inventor 郭彦春王志伟王瑞平刘春王晓龙
Owner 平顶山德源精细化学品有限公司