Preparation method of 3-methyl-4-isopropylaniline

A technology of isopropylaniline and toluidine, which is applied in the field of preparation of organic intermediates, can solve the problems of low production capacity, unsuitable for industrial production, and difficult availability of raw materials, etc., and achieves low pollution, few by-products, and high reaction efficiency. The effect of mild conditions

Active Publication Date: 2016-06-01
ZHEJIANG DINGLONG TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In existing reports, there are mainly two methods for preparing 3-methyl-4-isopropylaniline. The first method is to use m-toluidine as a raw material, under the effect of concentrated sulfuric acid, with isopropanol or 2 -Chloropropane carries out Friedel-Crafts reaction to obtain 3-methyl-4-isopropylaniline for isopropylating reagent, and this method is not only selectivity poor, and p

Method used

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  • Preparation method of 3-methyl-4-isopropylaniline

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Effect test

Embodiment 1

[0024] Add 1900.0g of sulfuric acid solution (95wt%) into the four-necked flask, stir and cool down to between 0 and 10°C, add 214.3g of m-toluidine dropwise, keep the temperature during the dropping process between 0 and 10°C, and control the drop for 2 hours. After the addition is completed, continue to stir for 30 minutes, and use it as component 1 for later use. Add 300.0 g of 2-chloropropane in another flask as component 2, and use a peristaltic pump to mix component 1 and component 2 at a ratio of 7:1. The flow rate (feed rate weight ratio) is simultaneously input into the T-type jet mixer and mixed rapidly at 20°C, and then pressed into the zirconia quartz reaction tube (microreactor) equipped with 6.0g of sulfuric acid, at 80-85 ℃ reaction to obtain the reaction solution of the alkylation reaction; the diameter of the quartz reaction tube is 2.5mm, the length of the tube is 2.0m, the residence time is 28s, and the particle size of the zirconia loaded with sulfuric acid ...

Embodiment 2

[0028] Add 2300.0g of sulfuric acid solution (80wt%) into the four-necked flask, stir and cool down to between 0 and 10°C, add 214.3g of m-toluidine dropwise, keep the temperature during the dropping process between 0 and 10°C, and control the drop for 2 hours. After the addition is completed, continue to stir for 30 minutes, and use it as component 1 for later use. Add 250g of isopropanol to another flask as component 2, and use a peristaltic pump to simultaneously mix components 1 and 2 at a flow rate of 10:1. Input it into a T-type jet mixer and mix rapidly at 30°C, then press it into a zirconia quartz reaction tube containing 6.0g of sulfuric acid, and react at 85-90°C to obtain the reaction solution of the alkylation reaction; the quartz reaction tube The pipe diameter is 5mm, the pipe length is 5m, the residence time is 40s, and the particle size of the zirconia loaded with sulfuric acid is 1.0mm; a 3L four-necked bottle is used to receive the reaction solution.

[0029]...

Embodiment 3

[0032] Add 2000.0g of sulfuric acid solution (85wt%) into the four-necked flask, stir and cool down to between 0 and 10°C, add 214.3g of m-toluidine dropwise, keep the temperature during the dropping process between 0 and 10°C, and control the drop for 2 hours. After the addition is completed, continue to stir for 30 minutes, and use it as component 1 for later use. In another flask, add 220 g of isopropanol as component 2, and use a peristaltic pump to mix component 1 and component 2 at a flow rate of 9:1 ( Feed rate (weight ratio) is simultaneously input into a T-type jet mixer for rapid mixing, and the mixing temperature is controlled at 25°C; then pressed into a zirconia quartz reaction tube containing 6.0g of sulfuric acid, and reacted at 70-75°C to obtain alkane The reaction solution of the radicalization reaction; the pipe diameter of the microreactor is 2.5mm, the pipe length is 2.0m, the residence time is 25s, and the particle size of the zirconia loaded with sulfuric ...

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Abstract

The invention relates to a preparation method of 3-methyl-4-isopropylaniline. The preparation method includes the following steps: (1) dissolving m-toluidine in sulfuric acid solution 50-98% in mass concentration as a component 1, then adding an isopropylation reagent into another container to serve as a component 2, simultaneously feeding the component 1 and the component 2 into a jet mixer with the flow rate of 5-10:1 to be mixed at the temperature of 10-35 DEG C, and then reacting at the temperature of 60-95 DEG C through a quartz reaction tube to obtain reaction solution for alkylation reaction; (2) subjecting the reaction solution obtained in the step (1) to separation and purification to obtain 3-methyl-4-isopropylaniline. The 3-methyl-4-isopropylaniline prepared through the method has the advantages of mild reaction condition, high yield, few by-products, less pollution and the like, and the problems of a lot of by-products, strict conditions and severe pollution in the preparation process of the 3-methyl-4-isopropylaniline in the prior art are solved effectively.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for preparing high-quality 3-methyl-4-isopropylaniline. Background technique [0002] 3-Methyl-4-isopropylaniline is an important organic intermediate widely used in medicine, dyes and other fields. At present, the method for preparing and synthesizing 3-methyl-4-isopropylaniline is not yet mature, and the existing methods for preparing 3-methyl-4-isopropylaniline are basically still in the stage of laboratory experiments. Can realize industrialized production. [0003] In existing reports, there are mainly two methods for preparing 3-methyl-4-isopropylaniline. The first method is to use m-toluidine as a raw material, under the effect of concentrated sulfuric acid, with isopropanol or 2 -Chloropropane carries out Friedel-Crafts reaction to obtain 3-methyl-4-isopropylaniline for isopropylating reagent, and this method is not only selectivity poor, and pr...

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C209/84C07C209/86C07C211/47
CPCC07C209/68C07C209/84C07C209/86C07C211/47
Inventor 秦振伟施云龙肖庆军刘琛胡晓峰
Owner ZHEJIANG DINGLONG TECH
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