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Preparation process of o-aminophenetole

A technology for the preparation of o-aminophenethyl ether, which is applied in the preparation of aminohydroxyl compounds, the preparation of organic compounds, organic chemistry, etc., can solve the problems that are not suitable for the development of green industry, the catalyst cannot be recycled, and the environmental protection problems are difficult to deal with. The effect of high product yield, high production capacity and stable product quality

Pending Publication Date: 2022-05-13
江苏普洛德化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process: on the one hand, the reaction process is carried out under high temperature and high pressure conditions, which is highly dangerous; on the other hand, the raw materials contain organic chlorine, and a certain amount of by-products will be produced during the reaction process, and environmental protection issues are difficult to deal with
[0004] At present, the phase-transfer catalytic synthesis process used in China is used to prepare o-aminophenethyl ether. This process uses o-nitrochlorobenzene and ethanol as raw materials, adopts a phase transfer catalyst, and then adds sodium hydroxide to generate o-nitrophenethyl ether, and then reduces it to obtain o-nitrophenethyl ether. Aminophenetole, although this process does not require high temperature and high pressure, the catalyst cannot be recovered, and a certain amount of pollution will still occur
Also not suitable for green industrial development requirements

Method used

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  • Preparation process of o-aminophenetole

Examples

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Effect test

Embodiment 1

[0027] A kind of preparation technology of o-aminophenethyl ether, described preparation technology comprises the steps:

[0028] (1) Catalytic hydrogenation: Add nitrobenzene, sulfuric acid, and ethanol mixture into the reaction kettle as raw material, add catalyst Pt-C, the equivalent diameter of the catalyst particles is 0.01-10.0mm, pass in hydrogen, the nitrobenzene in the mixture Hydrogenation and reduction reaction with hydrogen and ethanol will generate phenylethoxyamine, which will be transposed by sulfuric acid to generate o-aminophenethyl ether sulfate; the reaction temperature is 95-105°C, the hydrogen pressure is 0.3-0.5MPa, nitrobenzene, sulfuric acid , The consumption molar ratio of ethanol is 1:1.05:26;

[0029] (2) Solid-liquid separation: the mixed material in the step (1) is subjected to solid-liquid separation, the solid mixture enters the next step, and the liquid ethanol returns to the step (1) for mechanical application;

[0030] (3) Dissolving: the sol...

Embodiment 2

[0036] A kind of preparation technology of o-aminophenethyl ether, described preparation technology comprises the steps:

[0037] (1) Catalytic hydrogenation: Add nitrobenzene, sulfuric acid, and ethanol mixture into the reaction kettle as raw material, add catalyst Pt-C, the equivalent diameter of the catalyst particles is 0.01-10.0mm, pass in hydrogen, the nitrobenzene in the mixture Hydrogenation and reduction reaction with hydrogen and ethanol will generate phenylethoxyamine, which will be transposed by sulfuric acid to generate o-aminophenethyl ether sulfate; the reaction temperature is 95-105°C, the hydrogen pressure is 0.3-0.5MPa, nitrobenzene, sulfuric acid , The consumption molar ratio of ethanol is 1:1.05:20;

[0038] (2) Solid-liquid separation: the mixed material in the step (1) is subjected to solid-liquid separation, the solid mixture enters the next step, and the liquid ethanol returns to the step (1) for mechanical application;

[0039] (3) Dissolving: the sol...

Embodiment 3

[0045] A kind of preparation technology of o-aminophenethyl ether, described preparation technology comprises the steps:

[0046] (1) Catalytic hydrogenation: Add nitrobenzene, sulfuric acid, and ethanol mixture into the reaction kettle as raw material, add catalyst Pt-C, the equivalent diameter of the catalyst particles is 0.01-10.0mm, pass in hydrogen, the nitrobenzene in the mixture Hydrogenation and reduction reaction with hydrogen and ethanol will generate phenylethoxyamine, which will be transposed by sulfuric acid to generate o-aminophenethyl ether sulfate; the reaction temperature is 95-105°C, the hydrogen pressure is 0.3-0.5MPa, nitrobenzene, sulfuric acid , The consumption molar ratio of ethanol is 1:1.05:30;

[0047] (2) Solid-liquid separation: the mixed material in the step (1) is subjected to solid-liquid separation, the solid mixture enters the next step, and the liquid ethanol returns to the step (1) for mechanical application;

[0048] (3) Dissolving: the sol...

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Abstract

The invention relates to a preparation process of o-aminophenetole, which is characterized in that nitrobenzene, sulfuric acid and ethanol mixture are used as raw materials to prepare the o-aminophenetole, and the process is used for preparing the o-aminophenetole and ammonium sulfate through the steps of catalytic hydrogenation reduction, solid-liquid separation, water addition for dissolution, solid-liquid separation, acid-base neutralization, oil-water separation and the like. According to the method, nitrobenzene is adopted to replace o-nitrochlorobenzene, high temperature and high pressure are not needed, three wastes are not discharged, the method is a safe, environment-friendly and efficient o-aminophenetole synthesis process, and the purity of the obtained product reaches 99.90% or above and completely reaches the drug standard.

Description

technical field [0001] The invention relates to the technical field of fine chemical preparation, in particular to a preparation process of o-aminophenethyl ether. Background technique [0002] O-aminophenethyl ether is an important fine chemical intermediate, mainly used to make medicines and dyes. Because it can prevent the oxidation and deterioration of fat and protein during storage, it is also often used for the preservation of feed, food, vitamin A and vitamin E and other medicines. This product is widely used and has a large demand at home and abroad. The research and development of synthetic technology has received more and more attention and attention. [0003] The traditional synthesis route of o-aminophenethyl ether is as follows: using o-nitrochlorobenzene as raw material, placing the mixture of o-nitrochlorobenzene, ethanol and sodium hydroxide in a closed container, and under high temperature and pressure, to obtain o-nitrochlorobenzene Nitrophenethyl ether, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/84C07C213/00C07C213/10
CPCC07C213/00C07C213/10C07C239/20C07C217/84
Inventor 周龙根周鑫于冬英徐丹周宸萱
Owner 江苏普洛德化学科技有限公司
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