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Method for preparing 3,4-dimethoxy toluene under catalysis

A technology for the preparation of dimethoxytoluene and catalysis, which is applied in chemical instruments and methods, ether preparation, ester reaction to prepare ether, etc. It can solve problems such as long reaction time, not a production route, and gap in industrial application level, and achieve selectivity And the effect of high yield, good application prospect and low cost

Inactive Publication Date: 2014-04-16
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of reaction takes a long time and the separation of products is complicated, so it is not an economical production route
(4) Other catalysts such as CeO 2 , PdCl 2 (PhCN) 2 And Na Hg alloy etc., there are few reports about these catalysts being used to catalyze the preparation of 3,4-dimethoxytoluene;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 6.21g (0.045mol) of 4-methylguaiacol into a 100ml two-necked bottle, add 22.5ml of 2M NaOH solution, slowly heat up to 100°C under stirring, and introduce 0.045mol CH 3 Br, reacted for 1 h, the isolated yield of 3,4-dimethoxytoluene was 84.60%.

Embodiment 2

[0022] Weigh 6.21g (0.045mol) of 4-methylguaiacol in a 100ml two-necked bottle, add 22.5ml of 2M NaOH solution, stir and add 0.189g of catalyst (CH 3 ) 4 NBr, slowly warming up to 80°C under stirring, and feeding 0.09mol CH 3 Br, reaction 4h, the isolated yield of 3,4-dimethoxytoluene was 92.56%.

Embodiment 3

[0024] Take by weighing 6.21g (0.045mol) 4-methylguaiacol in 100ml two-necked bottle, add the NaOH solution of 22.5ml 2M, add 0.60g catalyst (C 4 h 9 ) 4 NBr, slowly warming up to 60°C under stirring, and feeding 0.15mol CH 3 Br, reaction 6h, the isolated yield of 3,4-dimethoxytoluene was 94.06%.

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PUM

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Abstract

The invention provides a method for preparing 3,4-dimethoxy toluene, which comprises the following steps of: alkalizing 4-methyl guaiacol with corresponding molar weight by using aqueous solution of inorganic alkali at certain concentration; heating alkalized 4-methyl guaiacol solution with stirring to the temperature of between 60 and 150 DEG C; and introducing monohalomethane into reaction liquid, reacting at the temperature of between 60 and 150 DEG C, cooling the reaction liquid after the reaction is finished, and directly separating to obtain a target product, namely the 3,4-dimethoxy toluene. The reaction speed and the yield of the product can be improved by adding an appropriate catalyst into the reaction liquid. The method for preparing the 3,4-dimethoxy toluene has the advantages of high selectivity and yield of the target product, and the like; in addition, the method is simple and has low cost and good application prospect.

Description

【Technical field】 [0001] The invention relates to the fields of fine chemical industry and organic synthesis, in particular to a method for catalytically preparing 3,4-dimethoxytoluene. 【Background technique】 [0002] 3,4-Dimethoxytoluene (3,4-Dimethoxytoluene), also known as 1,2-dimethoxy-4-methylbenzene (benzene, 1,2-dimethoxy-4-methyl-) is a synthetic fragrance and It is an important intermediate of pharmaceuticals and has a large market demand. At present, the main ways to catalyze the preparation of 3,4-dimethoxytoluene are: (1) with 3,4-dimethoxybenzyl alcohol, H 2 S and CO as raw materials, in the catalyst Co 2 (CO) 8 Under the action of conversion into 3,4-dimethoxytoluene. This type of reaction needs to be carried out under high temperature and high pressure, the reaction time is long, the product selectivity is poor, and the yield is low; and the poisonous gas H 2 S and CO are used as reaction reagents, which are easy to cause accidents such as poisoning and e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/205C07C41/16B01J31/02
Inventor 尹双凤欧阳强
Owner HUNAN UNIV