A kind of method for preparing 2,3,4,5-tetramethoxytoluene

A technology of tetramethoxytoluene and methoxy group, which is applied in the directions of ether preparation, ester reaction preparation of ether, chemical instruments and methods, etc., can solve the problems of difficult purification of products, low yield, and inconvenient industrial production.

Inactive Publication Date: 2015-11-18
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the raw materials used in the above synthetic routes are chemical synthesis products, the yield is not high, the product is not easy to purify, and it is not easy for industrial production.

Method used

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  • A kind of method for preparing 2,3,4,5-tetramethoxytoluene
  • A kind of method for preparing 2,3,4,5-tetramethoxytoluene
  • A kind of method for preparing 2,3,4,5-tetramethoxytoluene

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Experimental program
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Effect test

Embodiment 1

[0024] Double bromination reaction: In the reactor, add 138.2g of 4-methylguaiacol with a content of 99%, 600ml of dichloromethane, and 3g of PEG-600, stir and cool to about 0°C, and slowly and alternately add 30% hydrogen peroxide dropwise 260ml and 400g of 46% industrial hydrobromic acid solution, keep stirring at -5°C-15°C for reaction, drop it in about 8 hours, and then react for 1 hour. Stop stirring, after standing for 30 minutes, separate the upper layer of waste water and discard it; the lower layer of oil is stirred with 15ml×3 5% sodium carbonate solution for 1 hour to wash and neutralize each time to obtain the oil of lower layer pH=6. The dichloromethane solvent was distilled and recovered under boiling water conditions, and finally about 280g of a light red solid (that is, 2,3-dibromo-6-methoxy-4-methylphenol and 2,5-dibromo-6-methoxy -4-methylphenol).

[0025] Alkylation reaction: In the reactor, add 280g of the solid obtained in the double bromination reaction ...

Embodiment 2

[0028] Double bromination reaction: In the reactor, add 152.5g of 4-methylguaiacol with a content of 90%, 600ml of dichloromethane, and 3g of PEG-600, stir and cool to about 0°C, and slowly alternately add 30% hydrogen peroxide dropwise 260ml and 400g of 46% industrial hydrobromic acid solution, keep stirring at -5°C-15°C for reaction, drop it in about 8 hours, and then react for 1 hour. Stop stirring, after standing for 30 minutes, separate the upper layer of waste water and discard it; the lower layer of oil is stirred with 15ml×3 5% sodium carbonate solution for 1 hour to wash and neutralize each time to obtain the oil of lower layer pH=6. The dichloromethane solvent was distilled and recovered under boiling water conditions, and finally about 280.2 g of a light red solid (that is, 2,3-dibromo-6-methoxy-4-methylphenol and 2,5-dibromo-6-methoxy base-4-methylphenol).

[0029]Alkylation reaction: In the reactor, add 280.2 g of the solid obtained in the double bromination reac...

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Abstract

The invention provides a method for preparing 2, 3, 4, 5-tetramethoxytoluene by taking 4-hydroxy-3-methoxy-1-methyl-benzene as a raw material. The method comprises the process flows of brominating raw materials twice; then, carrying out hydrocarbonylation; and next, carrying out methoxymethylation to obtain 2, 3, 4, 5-tetramethoxytoluene. According to the invention, natural 4-hydroxy-3-methoxy-1-methyl-benzene extracted from biological oil is used as the raw material, so that the source of the raw material is relatively wide. The method is novel in ideal, simple and convenient in synthesis process, not high in requirements for reaction equipment and reaction conditions, relatively low in production cost and relatively high in industrial application value.

Description

technical field [0001] The invention belongs to the technical field of biomass utilization, and in particular relates to a method for preparing 2,3,4,5-tetramethoxytoluene. Background technique [0002] Coenzyme Q compounds are a class of vitamin substances and are commonly used drugs for the treatment of cardiovascular diseases, which have important physiological effects. At present, most of them are produced by chemical semi-synthetic methods. Among them, 2,3,4,5-tetramethoxytoluene is a very important pharmaceutical intermediate for the synthesis of coenzyme Q. [0003] 2,3,4,5-tetramethoxytoluene, English name 2,3,4,5-Tetramethoxytoluene, molecular formula C 11 h 16 o 4 , with a relative molecular mass of 212.24, has the structure shown in formula (1): [0004] [0005] The methods for synthesizing 2,3,4,5-tetramethoxytoluene reported in the current literature are as follows: (1) Using pyrogallic acid as raw material, through phenolic hydroxyl group forming methy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/205C07C41/16
CPCC07C41/16C07C41/22C07C43/2055C07C43/225C07C43/23
Inventor 朱锡锋朱昌朋李凯
Owner UNIV OF SCI & TECH OF CHINA
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