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A kind of preparation method of p-methoxybenzyl alcohol

A technology of methoxybenzyl alcohol and anisole, which is applied in the chemical industry, can solve the problems of by-product environmental pollution, low atom utilization rate, and long synthesis line, and achieve good stability, convenient recovery and recycling, and high activity Effect

Active Publication Date: 2021-10-19
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many defects in the above oxidation method: long synthesis line, low utilization rate of atoms, high production cost, serious environmental pollution caused by by-products, etc.

Method used

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  • A kind of preparation method of p-methoxybenzyl alcohol
  • A kind of preparation method of p-methoxybenzyl alcohol
  • A kind of preparation method of p-methoxybenzyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a round bottom flask, add anisole (1.0mol), paraformaldehyde (1.0mol), triazole chromium chloride salt ionic liquid functionalized mesoporous silicone immobilized transition metal copper (3.0g), heat up to 50°C and stirred for 10 hours. Cooling, filtering and separating the product and recovering the catalyst, the filtrate was washed with water, dried and rectified to obtain the product p-methoxybenzyl alcohol with a yield of 15.2%. LC-MS analysis results showed that the purity of p-methoxybenzyl alcohol was 94.8%.

Embodiment 2

[0025] In a round bottom flask, add anisole (1.0mol), paraformaldehyde (1.0mol), triazole tin chloride salt ionic liquid functionalized mesoporous organosilicon immobilized transition metal copper (3.0g), heat up to 60°C and stirred for 5 hours. Cooling, filtering and separating the product and recovering the catalyst, the filtrate was washed with water, dried and rectified to obtain the product p-methoxybenzyl alcohol with a yield of 19.5%. LC-MS analysis results showed that the purity of p-methoxybenzyl alcohol was 95.4%.

Embodiment 3

[0027] In a round bottom flask, add anisole (1.0mol), paraformaldehyde (1.0mol), triazole cupric chloride salt ionic liquid functionalized mesoporous organosilicon immobilized transition metal copper (4.0g), heat up to 60°C and stirred for 5 hours. Cooling, filtering and separating the product and recovering the catalyst, the filtrate was washed with water, dried and rectified to obtain the product p-methoxybenzyl alcohol with a yield of 18.3%. LC-MS analysis results showed that the purity of p-methoxybenzyl alcohol was 96.1%.

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Abstract

The invention discloses a preparation method of p-methoxybenzyl alcohol. After mixing anisole, paraformaldehyde and triazole ionic liquid functionalized mesoporous organosilicon-immobilized transition metal copper heterogeneous catalyst in a reaction vessel, the o C under stirring reaction for 1 to 12 hours, hydroxymethylation reaction occurs to obtain p-methoxybenzyl alcohol. The reaction system has the advantages of simple operation, mild reaction conditions, easy separation of the product catalyst, good recycling and reuse of the catalyst, and no risk to the ecological environment. It is an environmentally friendly method for preparing p-methoxybenzyl alcohol and is beneficial to industrial production.

Description

technical field [0001] The invention relates to a new method for preparing p-methoxybenzyl alcohol through the selective methylolation reaction of anisole catalyzed by triazole ionic liquid functionalized mesoporous organic silicon immobilized transition metal copper, and belongs to the technical field of chemical industry. [0002] technical background [0003] P-methoxybenzyl alcohol is an important fine chemical raw material, which is widely used in the synthesis of spices, medicines, pesticides, etc. At present, the industrial production methods of p-methoxybenzyl alcohol mainly include the Cannizzaro method and the catalytic hydrogenation method (Chem.AsianJ., 2009, 4(5):699-706; CN1994988A; JP2006088026). Although the Cannizzaro method has low requirements for equipment, it is highly corrosive to the equipment, consumes a lot of raw materials, produces many by-products, and produces a large amount of waste water, which is easy to pollute the environment; although the ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/26C07C43/23
CPCY02P20/584
Inventor 胡玉林谭津姚楠王龙张诺诺郑开波
Owner CHINA THREE GORGES UNIV
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