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Preparation method of 5-amino-2-methylphenol

A technology of methyl phenol and methyl aniline, which is applied in the field of preparation of chemical intermediates, can solve the problems of inability to obtain economic value and low yield, and achieve the effects of reducing environmental pollution, simple post-processing, and high product quality

Active Publication Date: 2018-04-27
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Although the raw materials of this method are cheap and easy to obtain, many iodine-containing reagents with high prices are used, and the yield is low. The reaction produces a large amount of spent alkali and waste acid, which leads to the inability to obtain higher economic value in actual production.

Method used

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  • Preparation method of 5-amino-2-methylphenol
  • Preparation method of 5-amino-2-methylphenol
  • Preparation method of 5-amino-2-methylphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1700kg of 50% sodium hydroxide solution in a 4800L autoclave, add 1850kg of ethanol solution containing 1000kg of 3-chloro-4-methylaniline, add 50kg of cuprous chloride, 15kg of copper powder, seal the reaction kettle, and replace it with nitrogen for 5 times. Raise the temperature to 175°C, keep warm for 4 hours, take samples for analysis, cool down after passing the test, recover ethanol under reduced pressure, filter it into an 8000L kettle, add 1450kg industrial hydrochloric acid to neutralize to weak acidity, add 2000L ethyl acetate to extract three times, and recover ethyl acetate under reduced pressure , to get the crude product.

[0032] Add 1000kg of ethanol to the crude product, raise the temperature to 60°C, add 50kg of activated carbon, stir for 1 hour, filter, cool down to 5°C to crystallize, and obtain 707kg of the product with a yield of 85.36% and a purity of 99.8%.

Embodiment 2～8

[0034] Concrete operation is with reference to embodiment 1, and the result after changing parameter condition is as shown in table 1:

[0035] Table 1

[0036]

[0037]

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PUM

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Abstract

The invention relates to a preparation method of 5-amino-2-methylphenol, comprising the steps of (1) adding an alkaline liquid into a high-pressure kettle, adding an alcohol solution containing 3-chloro-4-methylaniline, adding a catalyst, raising the temperature to 150-200 DEG C, and holding the temperature for reacting; (2) after reacting, cooling, recycling ethyl alcohol, and filtering to obtaina crude product; (3) purifying the crude product to obtain a fine product. The preparation method is simple; product post-processing is simple; low environmental pollution is caused; the prepared 5-amino-2-methylphenol has high quality; environment pollution is reduced at the premise of improved product quality, the product production is clean and environmentally friendly, and the product is moresuitable for batch production.

Description

technical field [0001] The invention relates to a preparation method of a chemical intermediate, in particular to a preparation method of high-quality 5-amino-2-methylphenol. Background technique [0002] 5-Amino-2-methylphenol has many important physical and chemical properties. It has very important applications in the chemical industry and is an indispensable chemical raw material. It is used in synthetic resins, dyeing, pigments, dyes, hair dyes, Medicines, pesticides, agrochemicals, photosensitive materials, explosives and many other fields, and because of its good disinfection and sterilization functions, it has also been widely used in shampoos, skin care products and other products in recent years. [0003] In the eighties of last century, people began to study the synthetic method of 5-amino-2-methylphenol, and the literature has reported several synthetic methods of 5-amino-2-methylphenol so far: [0004] 1. Using N-(4-dimethylaminomethyl-3-hydroxyphenyl)acetamide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/76C07C213/00C07C213/10
CPCC07C213/00C07C213/10C07C215/76
Inventor 潘志军叶炯英金宁人许惠钢张学
Owner ZHEJIANG DINGLONG TECH