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A kind of method of phenol dearomatization peroxyalkylation

A technology for aromatizing peroxane and phenol, applied in the direction of organic chemistry, etc., can solve the problem of late application of cobalt catalysts

Active Publication Date: 2022-04-29
HUBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with other transition metals, the application of cobalt catalysts in organic synthesis is relatively late

Method used

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  • A kind of method of phenol dearomatization peroxyalkylation
  • A kind of method of phenol dearomatization peroxyalkylation

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Embodiment 1

[0023] Add 0.4mmol 2,6-di-tert-butyl-p-cresol, 10mol% cobalt acetate tetrahydrate, 2eq silver carbonate, 5eq isobutanol, and 5mL tetrahydrofuran into a round-bottomed flask and heat in an oil bath at 40-80°C Reflux reaction, adjust the magnetic stirrer speed to 400-600 rpm, stop the reaction after 8-16 hours of reaction, let it cool down, use diatomaceous earth to absorb and filter impurities and wash with ethyl acetate three times, collect the filtrate for The crude product was obtained by distillation under reduced pressure. Finally, use ethyl acetate:petroleum ether=1:15 system to carry out column separation to obtain 2,6-di-tert-butyl-4-methyl-[4-(tetrahydrofuran peroxide)]-2,5-diene-1 - Cyclohexanone yellow solid pure product.

[0024] The structure of the product is determined by H NMR and C NMR: 1 H NMR (400MHz, CDCl 3 )δ6.62-6.50(m,2H),5.55(dd,J 1 =4Hz,J 1 =4Hz,1H),3.93-3.85(m,2H),2.00-1.76(m,3H),1.64-1.60(m,1H),1.36-1.33(m,3H),1.23(s,18H). 13 C NMR (100MHz, CDCl...

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Abstract

The present invention relates to a kind of method of phenol dearomatization peroxyalkylation, 2,6-di-tert-butyl p-cresol, cobalt acetate tetrahydrate, silver carbonate, isobutanol, tetrahydrofuran are added in the reactor, in Stir and heat in an oil bath at 40-80°C for 8 to 16 hours; after the reaction stops, let it stand for cooling, absorb and filter impurities with diatomaceous earth, wash with ethyl acetate three times, collect the filtrate and distill under reduced pressure to obtain the crude product ; Adopt ethyl acetate:petroleum ether=1:10 mobile relative to the gained crude product to carry out column separation, obtain 2,6-di-tert-butyl-4-methyl-[4-(tetrahydrofuran peroxide)]-2, 5‑Diene‑1‑cyclohexanone as a yellow solid pure product. The advantage of the synthesis method is that it uses cheap, easy-to-obtain and rich cobalt for catalysis, uses inorganic silver carbonate as an oxidant, has mild reaction conditions, simple process, and stable, safe and unprecedented products.

Description

technical field [0001] The present invention relates to a method for phenol dearomatization peroxyalkylation, in particular to a method for preparing 2,6-di-tert-butyl-4-methyl-[4-(tetrahydrofuran peroxide)]-2,5 - The method of diene-1-cyclohexanone. Background technique [0002] In the past, cobalt was widely used in the alloy industry. In recent years, due to the special catalytic effect of cobalt catalysts, researchers have attracted more and more attention. At present, many researchers have found that in some reactions, cobalt catalysts can replace some other noble metals. Compared with other transition metals, the application of cobalt catalysts in organic synthesis is relatively late. But in the next field of organic synthesis, cobalt will be more and more widely used as a new generation of catalysts. [0003] The peroxidation reaction is generally considered to be a reaction in which some substances react with ozone, and some very active substances react with hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/20
CPCC07D307/20
Inventor 张谦栗娟娟邓诗军解琳李栋
Owner HUBEI UNIV OF TECH