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One-pot process for synthesizing 1,2,3-trimethoxy-benzene by using o-vanillin

A technology of trimethoxybenzene and o-vanillin, applied in 1 field, achieves the effects of simple operation, low equipment requirements, and simple process steps

Inactive Publication Date: 2010-03-10
中化宁波(集团)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, there is no industrial application of ortho-vanillin through Dakin oxidation and remethylation.

Method used

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  • One-pot process for synthesizing 1,2,3-trimethoxy-benzene by using o-vanillin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In actual production, 200 kilograms of o-vanillin, 52 kilograms of sodium hydroxide, and 500 kilograms of water were put into the reaction kettle in turn for stirring. After stirring and mixing evenly, 2200 kilograms of 3% hydrogen peroxide were added dropwise. As the dropwise addition proceeded, the reaction was slightly exothermic, and the color of the reaction solution gradually became darker. After the dropwise addition, keep warm until the reaction is complete. The end point of the reaction was judged by thin-layer chromatography (TLC), and the developer was 4 / 6 ethyl acetate / petroleum ether, and the reaction was considered complete until the raw material point completely disappeared. After the reaction was completed, 415 kilograms of dimethyl sulfate and 440 kilograms of 30% sodium hydroxide aqueous solution were added dropwise, and the rate of addition of the two was controlled so that the pH in the still was maintained at 9~10, and the temperature was controlled...

Embodiment 2

[0021] In actual production, 200 kilograms of o-vanillin, 67 kilograms of sodium hydroxide, and 533 kilograms of water were put into the reaction kettle successively for stirring. After stirring and mixing evenly, 2340 kilograms of 3% hydrogen peroxide were added dropwise. As the dropwise addition proceeded, the reaction was slightly exothermic, and the color of the reaction solution gradually became darker. After the dropwise addition, keep warm until the reaction is complete. The end point of the reaction was judged by thin-layer chromatography (TLC), and the developer was 4 / 6 ethyl acetate / petroleum ether, and the reaction was considered complete until the raw material point completely disappeared. After the reaction was completed, 332 kilograms of dimethyl sulfate and 350 kilograms of 30% sodium hydroxide aqueous solution were added dropwise, and the rate of addition of the two was controlled so that the pH in the still was maintained at 9~10, and the temperature was contr...

Embodiment 3

[0023] In actual production, 200 kg of ortho-vanillin, 40 kg of sodium hydroxide, and 400 kg of water were put into the reaction kettle in turn for stirring. After stirring and mixing evenly, 1800 kg of 3% hydrogen peroxide was added dropwise. As the dropwise addition proceeded, the reaction was slightly exothermic, and the color of the reaction solution gradually became darker. After the dropwise addition, keep warm until the reaction is complete. The end point of the reaction was judged by thin-layer chromatography (TLC), and the developer was 4 / 6 ethyl acetate / petroleum ether, and the reaction was considered complete until the raw material point completely disappeared. After the reaction was completed, 663 kilograms of dimethyl sulfate and 700 kilograms of 30% sodium hydroxide aqueous solution were added dropwise, and the rate of addition of the two was controlled so that the pH in the still was maintained at 9~10, and the temperature was controlled between 35~40°C. After ...

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Abstract

The invention provides a synthesis process of 1,2,3-trimethoxy-benzene, which is characterized by comprising: putting o-vanillin and sodium hydroxide in a reaction kettle; dripping hydrogen peroxide at room temperature; subjecting the mixture to Dakin oxidation; dripping dimethyl sulfate and industrial caustic soda liquid; after the completion of the reaction, performing extraction with methylbenzene; concentrating and recovering the methylbenzene; and adding ethanol-water recrystallization to obtain the refined 1,2,3-trimethoxy-benzene. The synthesis process of the 1,2,3-trimethoxy-benzene isprocess sequence, low in equipment requirement, simple in operation, high in product yield and quality, and suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis and preparation method of an organic compound, in particular to a preparation method of 1,2,3-trimethoxybenzene. Background technique [0002] 1,2,3-Trimethoxybenzene is widely used in organic synthesis and pharmaceutical industry, and it is an important intermediate in the production of various drugs. In the past, this product was produced by using the traditional Chinese medicine gallnut and imported tara powder. Patent application 200510018690.4 discloses a method for preparing 1,2,3-trimethoxybenzene by using pyrogallic acid, and patent application 200610030549.0 discloses a method for producing 1,2,3-trimethoxybenzene by using tea bar maple leaves method. At present, there is no industrial application of the production method of o-vanillin through Dakin oxidation and remethylation. Contents of the invention [0003] The purpose of this invention is to provide a kind of synthesis technique of 1,2,3-trimetho...

Claims

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Application Information

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IPC IPC(8): C07C43/205C07C41/01
Inventor 王忠美李斌陈令武王金钢林邦平杨建军
Owner 中化宁波(集团)有限公司
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