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Preparation method of m-ethylaniline

A technology for ethylaniline and nitroacetophenone, which is applied in the directions of preparing amino compounds from amines, preparing hydrazones, organic chemistry, etc., can solve problems such as heat amplification, difficulty in controlling safety, unfavorable industrial production, etc., and achieves easy operation, high yield effect

Inactive Publication Date: 2022-02-01
苏州精杰瑞生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method reported in the literature mainly uses cheaper m-nitroacetophenone as a raw material to produce products through the Huang Minglong reaction in one step. The reaction system will release a large amount of gas and heat in an instant, and the safety is difficult to grasp, which is not conducive to industrial production.

Method used

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  • Preparation method of m-ethylaniline
  • Preparation method of m-ethylaniline
  • Preparation method of m-ethylaniline

Examples

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Embodiment 1

[0021] A preparation method for m-ethylaniline, comprising the following steps:

[0022] Step 1. Add 80g of m-nitroacetophenone into a 500ml three-necked flask, add 160ml of methanol, heat to about 65°C, then add 36g of hydrazine hydrate, and continue to heat and reflux for 1.5 hours; after the reaction is completed, the reaction solution is directly used in the following one step reaction;

[0023] Step 2: Add the reaction solution into the hydrogenation reactor, add 0.2g of palladium carbon, pressurize the hydrogen to 0.25mpa, and react at 50-60°C for 2 hours, and the reaction ends;

[0024] Step 3. Keep the reactant obtained in step 2 warm at 45-55°C, let it stand, and extract the supernatant; add it to a 500ml three-necked bottle, add 40g of potassium hydroxide to it for heating reaction, heat and keep the reaction at 90°C to No fraction distilled out, continue to heat up to 120°C to react until no fraction distilled out, continue to heat up to 150°C to react, and the rea...

Embodiment 2

[0034] A preparation method for m-ethylaniline, comprising the following steps:

[0035] Step 1. Add 80g of m-nitroacetophenone into a 500ml three-necked flask, add 160ml of methanol, heat to about 65°C, then add 36g of hydrazine hydrate, and continue to heat and reflux for 1.5 hours; after the reaction is completed, the reaction solution is directly used in the following one step reaction;

[0036] Step 2: Add the reaction solution into the hydrogenation reactor, add 0.2g of palladium carbon, pressurize the hydrogen to 0.25mpa, and react at 50-60°C for 2 hours, and the reaction ends;

[0037] Step 3. Keep the reactant obtained in step 2 warm at 45-55°C, let it stand, and extract the supernatant; add it to a 500ml three-necked bottle, add 40g of potassium hydroxide to it for heating reaction, heat and keep the reaction at 90°C to No fraction distilled out, continue to heat up to 120°C to react until no fraction distilled out, continue to heat up to 150°C to react, and the rea...

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Abstract

The invention discloses a preparation method of m-ethylaniline, which comprises the following steps: step 1, adding 80g of m-nitroacetophenone into a 500ml three-necked flask, adding 160ml of methanol, heating to about 65 DEG C, then adding 36g of hydrazine hydrate, and continuing a heating reflux reaction for 1.5 hours; after the reaction is finished, directly using reaction liquid for next-step reaction; step 2, adding the reaction liquid into a hydrogenation reaction kettle, adding 0.2 g of palladium on carbon, pressurizing with hydrogen to 0.25 mpa, reacting at 50-60 DEG C for 2 hours, and ending the reaction; and 3, keeping the temperature of the reactant obtained in the step 2 at 45-55 DEG C, performing standing, and extracting a supernatant. The preparation method of m-ethylaniline adopts a new route, the new route decomposes the reaction into three-step reaction, each step is safe and controllable, the yield is high, the first two steps in the three-step reaction do not need post-treatment operation, and the operation is simple and convenient. The method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of intermediate synthesis, in particular to a preparation method of m-ethylaniline. Background technique [0002] As an important intermediate of Cerestat and Paquinimod, m-ethylaniline has high economic value. [0003] The method reported in the literature mainly uses cheaper m-nitroacetophenone as a raw material to produce products through the Huang Minglong reaction in one step. This reaction system will release a large amount of gas in an instant and generate a large amount of heat. It is difficult to control the safety and is not conducive to industrial production. Contents of the invention [0004] For the problems mentioned in the background technology, the purpose of the present invention is to provide a kind of preparation method of m-ethylaniline, to solve the problems mentioned in the background technology. [0005] Above-mentioned technical purpose of the present invention is achieved through ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C211/47
CPCC07C209/68C07C249/16C07C211/47C07C251/86
Inventor 闫永平胡海威丁靓
Owner 苏州精杰瑞生物科技有限公司
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