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Preparation method of 3-methyl-4-isopropylphenol

A technology of isopropylphenol and isopropylaniline, which is applied in the field of highly selective preparation of 3-methyl-4-isopropylphenol, can solve the problems of low phenol preparation yield, many by-products, and high yield , to achieve the effect of less pollution, less by-products and high yield

Inactive Publication Date: 2013-04-17
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of this invention is to provide a kind of preparation method of 3-methyl-4-isopropyl phenol, use this method to directionally synthesize 3-methyl-4-isopropyl phenol, have the characteristics of high yield and little pollution, solve the problem of The preparation yield of 3-methyl-4-isopropylphenol is low and the problem of many by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation of 3-methyl-4-isopropylaniline

[0024] Add 2143.0g of sulfuric acid aqueous solution (85wt%) into the four-necked flask, stir and cool down to between 0~10°C, add m-toluidine 214.3g (2mol) dropwise, and keep the temperature during the dropping process between 0~10°C. Control the dropwise addition for about 2 hours. After the addition is completed, continue to stir for 30 minutes, then raise the temperature to 75~80°C, and start adding 120.2g of isopropanol dropwise after raising the temperature to 75°C. After about 3 hours, the addition is completed, and the reaction is kept for 3~5 hours. , GC detection, stop the reaction when the content of 3-methyl-4-isopropylaniline in the reaction solution is controlled between 40-45%, cool down in an ice-water bath to 10-30°C, and then add ammonia water with a mass concentration of 25% dropwise Adjust the reaction solution to pH=7~9, filter to remove solid salt, rinse the filter cake with 100ml ethyl...

Embodiment 2

[0034] Embodiment 2: the preparation of 3-methyl-4-isopropylaniline

[0035] Add 1845.0g sulfuric acid aqueous solution (85wt%) into the four-necked flask, stir and cool down to 0~10℃, add m-toluidine 214.3g (2mol) dropwise, keep the temperature during the dropping process at 0~10℃, Control the dropwise addition for about 3 hours. After the addition is complete, continue to stir for 60 minutes, then raise the temperature to 75~80°C, and start adding 96g of isopropanol dropwise after raising the temperature to 80°C. After about 3h, the addition is completed, and the temperature is kept for 3~5h. , GC detection, stop the reaction when the total amount of the product is controlled between 40~45%, cool down to 20-30°C in an ice-water bath, then dropwise add ammonia solution with a mass concentration of 25% to adjust the reaction solution to pH=7~9, filter Remove the solid salt, rinse the filter cake with 200ml ethyl acetate, combine the rinsing liquid and filtrate and extract with...

Embodiment 3

[0037] Embodiment 3: the preparation of 3-methyl-4-isopropylaniline

[0038] Add 1400.0g sulfuric acid aqueous solution (85wt%) into the four-necked flask, stir and cool down to 0~10°C, add m-toluidine 214.3g (2mol) dropwise, and keep the temperature during the dropping process at 0~10°C. Control the dropwise addition for about 2 hours. After the addition is completed, continue to stir for 30 minutes, then raise the temperature to 75~80°C, and start adding 72g of isopropanol dropwise after raising the temperature to 75°C. After about 3 hours, the addition is completed, and the reaction is kept for 3~5 hours. GC detection, stop the reaction when the total amount of product is controlled between 40-45%, cool down in an ice-water bath to 15-30°C, then dropwise add ammonia solution with a mass concentration of 25% to adjust the reaction solution to pH=7~9, filter to remove Solid salt, the filter cake was rinsed with 100ml ethyl acetate, the rinsing solution and the filtrate were c...

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PUM

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Abstract

The invention discloses a preparation method of 3-methyl-4-isopropylphenol. The method comprises the following steps of: (1) dissolving m-toluidine into sulfuric acid to react with an isopropylation reagent to obtain 3-methyl-4-isopropylaniline, wherein the isopropylation reagent is isopropanol, propylene or 2-chloropropane; (2) hydrolyzing the 3-methyl-4-isopropylaniline to obtain a reaction solution containing the 3-methyl-4-isopropylphenol, wherein the hydrolysis is diazo hydrolysis or high-temperature high-pressure hydrolysis by using the sulfuric acid as a solvent; and (3) distilling the reaction solution containing the 3-methyl-4-isopropylphenol and performing solvent refining to obtain needle-like crystalline 3-methyl-4-isopropylphenol. The method disclosed by the invention has the characteristics of mild reaction condition, high yield, few by-products and little pollution; and the preparation method effectively solves difficulties such as many by-products, severe condition and great pollution in the existing preparation process of the 3-methyl-4-isopropylphenol.

Description

(1) Technical field [0001] The invention relates to a highly selective preparation method of 3-methyl-4-isopropylphenol. (2) Background technology [0002] 3-Methyl-4-isopropylphenol is an important cosmetic raw material, which has the functions of sterilization, antiperspirant and deodorant, and is widely used in shampoo, soap, hand sanitizer, toothpaste and other personal hygiene products and cosmetics. It is a good substitute for triclosan and other old-generation fungicides. It has the characteristics of safety, low toxicity, skin-friendly, easy degradation and less environmental pollution. This compound has been widely adopted by major cosmetic companies, and its scope of use is gradually expanding, and its usage is also increasing year by year. But how to obtain the high-purity substance is still a difficult problem encountered in the product development and promotion process. [0003] The more common preparation method for preparing 3-methyl-4-isopropyl phenol now m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/05
Inventor 秦振伟施云龙肖庆军刘琛
Owner ZHEJIANG DINGLONG TECH
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