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Method for preparing 4-methylcatechol by using methanol and magnesium

A technology of methyl catechol and magnesium methylate, applied in the field of 4-methyl catechol, can solve the problems of large amount of solvent, large amount of waste water, increased production cost and waste water, etc., and achieves mild reaction conditions and simple process route. Effect

Inactive Publication Date: 2017-09-29
HUNAN NORMAL UNIVERSITY
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Problems solved by technology

The yield and reaction steps of this method are similar to those of the Fries rearrangement method. Since the hydrolysis of anhydrous magnesium chloride is milder than that of anhydrous aluminum trichloride, no hydrogen chloride gas is generated, but there are also shortcomings such as a large amount of solvent required for the reaction and a large amount of waste water. , in addition, the recovery of triethylamine increases the production cost and the generation of waste water

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  • Method for preparing 4-methylcatechol by using methanol and magnesium

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example 1

[0005] Magnesium powder (14.4 g, 0.6 mol) was put into a four-necked reaction bottle filled with 200 ml of methanol, and the electric stirring was turned on, a large number of bubbles were generated in the bottle, and the temperature rose to 61 °C. After 2h, the solution turned into a milky white suspension. P-cresol (108 g, 1.0 mol) was added to the reaction flask, methanol was distilled off after 50 min, and 200 ml of toluene was added after the reaction liquid became thick. Raise the temperature, and when the internal temperature reaches 95°C, add paraformaldehyde (90 g, 3.0 mol) in batches, change the device to a distillation device, and evaporate low-boiling substances. After 30 minutes, almost no fractions are distilled, and remove the distillation device , continue to react for 2.5h, followed by TLC point plate, p-cresol reacted completely. Stop heating, and when the internal temperature drops to 65°C, adjust the pH to 1 with 18.5% hydrochloric acid. After standing st...

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Abstract

The invention relates to a method for preparing 4-methylcatechol by using methanol and magnesium. 4-methylcatechol is an important basic chemical raw material, many document reports on the synthesis processes of 4-methylcatechol exist, but the processes can not easily implement industrialization. The method comprises the following steps: carrying out a reaction on the raw material paracresol with methanol and magnesium to synthesize magnesium p-cresylate, synthesizing 3-methylsalicylaldehyde from the magnesium p-cresylate, and carrying out oxidation by using oxydol to synthesize the 4-methylcatechol. In terms of the paracresol, the total reaction yield can reach 80%. Compared with the existing documents, the method has the advantages of simple process route, mild reaction conditions, high reaction yield and the like, and is suitable for industrialization.

Description

technical field [0001] The present invention adopts p-cresol as raw material, prepares p-cresyl magnesium by reacting with metal magnesium methoxide, reacts p-cresyl magnesium and paraformaldehyde to prepare 3-methyl salicylaldehyde, and oxidizes 3-methyl salicylaldehyde with hydrogen peroxide to produce To obtain 4-methylcatechol, calculated as p-cresol, the total reaction yield can reach 80%. Compared with the existing literature, the method has the advantages of simple process route, mild reaction conditions, high reaction yield and suitability for industrialization. Background technique [0002] 4-Methylcatechol is an important basic chemical raw material, and its synthesis method has been reported in many literatures. According to the literature review, its synthesis method can be roughly divided into the following categories: 1. Liquefied lignin method. This method uses high temperature (370-380 o C) and high pressure (200-210 atm), use ferric oxide, nickel oxide and...

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Application Information

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IPC IPC(8): C07C37/60C07C39/08
CPCC07C37/60C07C37/66C07C45/45C07C39/235C07C47/565C07C39/08
Inventor 刘建兵祝岱桢黄雅丹
Owner HUNAN NORMAL UNIVERSITY
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