2,3-dimethoxy-5-methyl-1,4-benzoquinone ú¿ó±ú®preparation method

A technology of trimethoxytoluene and dimethoxy, which is applied in 2 fields, can solve the problems of large corrosion of industrial equipment, unsuitable for large-scale industrial production, corrosion of industrial equipment, etc., and achieves the effects of less environmental pollution, easy recycling and application, and simple operation.

Inactive Publication Date: 2004-11-10
FUDAN UNIV
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  • Application Information

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Problems solved by technology

Japanese Patent (Japanese Patent Application No. 54-106440) describes the use of 60% H 2 o 2 A method of directly oxidizing 3,4,5-trimethoxytoluene (II) to prepare (I) at 0°C, but this method requires a large amount of strong acid: trifluoroacetic acid as a catalyst, which is not only expensive but also corrosive to industrial equipment Seriously, the yield is not high (68%)
Japanese Patent (Japanese Patent Application No. 56-75450) also describes the use of (NH 4 ) 2 S 2 o 8 The method of preparing (I) by direct oxidatio

Method used

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  • 2,3-dimethoxy-5-methyl-1,4-benzoquinone ú¿ó±ú®preparation method
  • 2,3-dimethoxy-5-methyl-1,4-benzoquinone ú¿ó±ú®preparation method
  • 2,3-dimethoxy-5-methyl-1,4-benzoquinone ú¿ó±ú®preparation method

Examples

Experimental program
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Embodiment

[0014] (1) Preparation of 2,3,4-trimethoxy-6-methyl-benzaldehyde

[0015] Embodiment (1): 250ml dry three-necked flask is placed in ice-water bath, adds 120 grams (0.66mol) of 3,4,5-trimethoxytoluene and 76ml (72g, 0.99mol) of dimethylformamide, mechanical stirring Let it dissolve completely. Slowly add 72 ml of phosphorus oxychloride (120 g, 0.78 mol) dropwise thereto, stir at 30°C for 2 h after the addition, and then raise the temperature to 90°C for 1 h to complete the reaction to obtain a brown-red viscous liquid. Slowly pour it into ice water, add 2N aqueous sodium hydroxide solution under stirring until the solution is weakly alkaline, collect the precipitated white solid, wash with water, and dry in vacuo to obtain white solid 2,3,4-trimethoxy-6-methanol Base-benzaldehyde 133g, yield 96%, Mp: 61°C.

[0016] Example (2): A 100ml dry three-necked flask was placed in an ice-water bath, 12g (0.065mol) of 3,4,5-trimethoxytoluene and 15ml of dimethylformamide were added, an...

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PUM

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Abstract

The invention relates to a process for preparing 2,3-dimethoxy-5- methyl-1,4- benzophenone (I) by subjecting raw material 3,4,5-trimethoxytoluene (II) first with phosphorus oxytrichloride and N,N-dimethyl formamide to Vilsmeier reaction, obtaining 2,3,4-trimethoxyl-6- methyl- benzaldehyde (III) by introducing aldehydo onto phenyl ring, and oxidizing (III) into phenol (IV) with H2O2 at the presence of small amount organic acid catalysis at room temperate.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and is a preparation method of 2,3-dimethoxy-5-methyl-1,4-benzoquinone (I) [0002] Background technique [0003] 2,3-dimethoxy-5-methyl-1,4-benzoquinone (I) is a synthetic coenzyme Q series compound (CoQ 1-10 ) is an important starting material. Japanese Patent (Japanese Patent Application No. 54-106440) describes the use of 60% H 2 o 2 A method of directly oxidizing 3,4,5-trimethoxytoluene (II) to prepare (I) at 0°C, but this method requires a large amount of strong acid: trifluoroacetic acid as a catalyst, which is not only expensive but also corrosive to industrial equipment Seriously, the yield is not high (68%). Japanese Patent (Japanese Patent Application No. 56-75450) also describes the use of (NH 4 ) 2 S 2 o 8 (II) is directly oxidized to prepare (I), but this method still needs to be catalyzed and extracted with a large amount of concentrated sulfuric acid, the operation ...

Claims

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Application Information

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IPC IPC(8): C07C46/00C07C50/28
Inventor 楚勇陈芬儿
Owner FUDAN UNIV
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