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2-(4-methylphenyl)propionic acid syntehsis method

A technology of methyl phenyl and synthetic methods, which is applied in the direction of chemical instruments and methods, carboxylate preparation, carboxynitrile preparation, etc., can solve the problems of many types of chemical raw materials, many organic solvents, and large amounts of waste water, and achieve easy Realize the effects of industrialization, stable reaction and short process route

Active Publication Date: 2015-03-11
柳州丰康泰科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses many types of chemical raw materials, many organic solvents, a large amount of waste water, and waste residues.

Method used

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  • 2-(4-methylphenyl)propionic acid syntehsis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1: A kind of synthetic method of 2-(4-methylphenyl) propionic acid, comprises the following steps:

[0056] (1) Chlorination reaction: the preparation of p-methylbenzyl chloride (compound Ⅰ), the specific operation steps are as follows:

[0057] (1) Add 250L of p-xylene liquid into the reactor, fill the tail gas suction tank of the reactor with water, and the water level is 40-70%. Turn on the reaction kettle to stir, heat the p-xylene to about 75°C and keep it at a constant temperature, turn on a 100W blue light with a wavelength of 450nm to irradiate, and slowly introduce chlorine gas under light conditions to react (flow rate 5-10m 3 / hr), and follow-up analysis to monitor the product situation.

[0058] (2) Analysis results When p-methyl benzyl chloride is about 30% and other chlorides are detected, such as p-dimethyl chlorobenzene, p-dichloro benzyl or polychloride, close the chlorine gas valve and stop heating , turn off the light source and stop the ...

Embodiment 2

[0090] Example 2: A kind of synthetic method of 2-(4-methylphenyl)propionic acid, the specific operation steps of step (1), step (2) and step (4) are the same as those in Example 1, the difference lies in step (3) Methylation reaction: the preparation of 2-(4-methylphenyl)propionitrile (compound Ⅲ), the specific operation steps are as follows:

[0091] (1) Add 30kg (0.229kmol) of p-tolueneacetonitrile and 150kg (1.665kmol) of dimethyl carbonate into the reactor respectively from the feeding product, and then add 2.1kg of triethanolamine from the feeding port of the basic substance.

[0092] (2) Pressure test: Use nitrogen to test the pressure, the pressure is about 3Mpa, and there is no leakage. Slowly release pressure and discharge nitrogen. Close the valve.

[0093] (3) Turn on stirring and set the stirring speed.

[0094] (4) Turn on the exhaust gas cooler to circulate cooling water.

[0095] (5) Turn on the reactor heating device. Gradually raise the temperature and...

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PUM

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Abstract

The invention relates to a synthesis method of a fine chemical product 2-(4-methylphenyl)propionic acid. According to the method, para-xylene is adopted as a raw material, and a chlorination reaction is carried out, such that a compound I which is p-methylbenzyl chloride is obtained; p-methylbenzyl chloride is subjected to a nitrilation reaction, such that a compound II which is p-methylbenzyl cyanide is adopted; p-methylbenzyl cyanide is subjected to methylation, such that a compound III which is 2-(4-methylphenyl)propionitrile is obtained; and 2-(4-methylphenyl)propionitrile is subjected to hydrolysis acidification, such that a compound IV which is 2-(4-methylphenyl)propionic acid is obtained. The method provided by the invention has the advantages of short process route, low three-waste discharge, low environment pollution, no solid waste production during reaction processes, relatively low production cost, less chemical substances used during reaction processes, less raw material types, easy-to-obtain raw materials, simple operation, high yield, relatively mild process conditions, and the like.

Description

technical field [0001] The invention relates to a synthesis method of a fine chemical product 2-(4-methylphenyl)propionic acid. Background technique [0002] 2-(4-methylphenyl)propionic acid, the structure test (Ⅳ) is: [0003] [0004] It is an extremely important non-steroidal anti-inflammatory drug profen drug intermediate, and there are some reports on its synthesis method literature, mainly as follows: [0005] "Study on the Rearrangement Synthesis Process of Loxoprofen Sodium" by Chen Fen'er et al. ("China Pharmaceutical Industry Journal" 1998, 29 (12), 531-533) discloses using toluene as the starting material, toluene and 2-chloro Propionyl chloride was synthesized by Friedel-Crafts acylation, ketalization, 1, 2-aryl rearrangement (rearrangement under the catalysis of Lewis acid zinc salt, etc.), hydrolysis and other steps to synthesize compound IV (2-(4-methylphenyl ) propionic acid). The synthetic route is simple and convenient, but there are many types of che...

Claims

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Application Information

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IPC IPC(8): C07C51/08C07C57/30
CPCC07C17/14C07C51/02C07C51/41C07C253/14C07C253/30C07C57/30C07C255/33C07C22/04
Inventor 王欣荣刘仁华覃秀凤覃春极袁捷才曾蔚何艳杨志华黄婷叶美玲蒋薇薇韦静黄景春覃新善欧阳葭韦志鑫闭武勤
Owner 柳州丰康泰科技有限公司
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