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Method for synthesizing 2,3,5-trimethylbenzoquinone and 2,3,5-trimethylhydroquinone

A technology of trimethylhydroquinone and trimethylbenzoquinone, which is applied in chemical instruments and methods, preparation of quinone oxides, preparation of organic compounds, etc., can solve the problems of high technical requirements and short process, and achieve simple steps, The effect of low equipment requirements and few by-products

Inactive Publication Date: 2011-10-19
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process has the advantages of short process, high product yield, and low pollution, but the process requires high technology

Method used

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  • Method for synthesizing 2,3,5-trimethylbenzoquinone and 2,3,5-trimethylhydroquinone
  • Method for synthesizing 2,3,5-trimethylbenzoquinone and 2,3,5-trimethylhydroquinone
  • Method for synthesizing 2,3,5-trimethylbenzoquinone and 2,3,5-trimethylhydroquinone

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 2g of 2,3,6-trimethylphenol in 20ml of acetonitrile, add it into a three-necked flask, weigh 0.1g of Cu-SBA-15 mesoporous molecular sieve into the flask, heat it in a water bath to 50°C, add 3ml of 30% Hydrogen peroxide, start timing, react for 3h. The final conversion rate was 6.6%, the selectivity to TMBQ was 62.0%, and the selectivity to TMHQ was 18.9%.

Embodiment 2

[0028] Dissolve 2g of 2,3,6-trimethylphenol in 20ml of acetonitrile, add it into a three-necked flask, weigh 0.1g of Cu-SBA-15 mesoporous molecular sieve into the flask, heat it in a water bath to 60°C, add 3ml of 30% Hydrogen peroxide, start timing, react for 3h. The final conversion rate was 12.0%, the selectivity to TMBQ was 59.4%, and the selectivity to TMHQ was 18.9%.

Embodiment 3

[0030] Dissolve 2g of 2,3,6-trimethylphenol in 20ml of acetonitrile, add it into a three-necked flask, weigh 0.1g of Cu-SBA-15 mesoporous molecular sieve into the flask, heat it in a water bath to 70°C, add 3ml of 30% Hydrogen peroxide, start timing, react for 3h. The final conversion rate was 25.9%, the selectivity to TMBQ was 54.3%, and the selectivity to TMHQ was 21.9%.

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Abstract

The invention provides a method for synthesizing 2,3,5-trimethylbenzoquinone and 2,3,5-trimethylhydroquinone. In the method, the 2,3,5-trimethylbenzoquinone and the 2,3,5-trimethylhydroquinone are prepared by oxidizing reaction at the temperature of between 50 and 80 DEG C in the presence of a Cu-SBA-15 mesoporous molecular sieve serving as a catalyst, H2O2 serving as an oxidant and acetonitrile serving as a solvent. In the method, the reaction process is simple, and the equipment requirement is low; the Cu-SBA-15 mesoporous molecular sieve is used as the catalyst, contributes to the dispersion of products and is easy to separate; and the H2O2 is used as the oxidant, and the byproduct is H2O, so that the method is environment-friendly.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis technology, in particular to the synthesis technology of 2,3,5-trimethylbenzoquinone (TMBQ) or 2,3,5-trimethylhydroquinone (TMHQ). Background technique [0002] 2,3,5-Trimethylhydroquinone is an important intermediate for the synthesis of vitamin E. 2,3,5-Trimethylbenzoquinone can be reduced to 2,3,5-Trimethylhydroquinone. Vitamin E is widely used in medicine, health products, food, cosmetics, animal husbandry and other fields. [0003] At present, the synthetic methods of 2,3,5-trimethylhydroquinone mainly contain the following types: [0004] (1) Trimethylbenzene method [0005] Trimethylbenzene undergoes sulfonation, nitration, and hydrogenation reduction to 1,2,4-trimethyl-3,6-diaminobenzenesulfonic acid, and then oxidizes to 2,3,5-trimethylbenzoquinone , and finally hydrogenation reduction to obtain 2,3,5-trimethylhydroquinone. [0006] [0007] This process route has the ad...

Claims

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Application Information

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IPC IPC(8): C07C50/02C07C46/06C07C39/08C07C37/00
Inventor 孔黎明周涛菅盘铭
Owner YANGZHOU UNIV
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