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Preparation method of 2-phenylpropionic acid

A technology of phenylpropionic acid and phenylpropanil, applied in the chemical field, can solve the problems of complex preparation steps, difficult conditions, high control and high cost, and achieve the effect of simplified process and simple equipment

Active Publication Date: 2014-02-05
CHANGZHOU TIANHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing 2-phenylpropionic acid products are usually prepared from acetophenone as a raw material by first reducing chlorine under high pressure hydrogenation and then by chlorination. The preparation steps of this method are complicated, the conditions are difficult to control, and the cost is high

Method used

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  • Preparation method of 2-phenylpropionic acid
  • Preparation method of 2-phenylpropionic acid
  • Preparation method of 2-phenylpropionic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In a 500ml reaction bottle, put 100g of styrene and 300g of hydrochloric acid solution with a mass concentration of 20%, at a temperature of 35-37°C, stir and react for 10 hours. After sodium sulfate was dried for 2 hours, the concentration of the oil layer was weighed to be 97.8%, and the content of α-chloroethylbenzene analyzed by gas chromatography was 98.67%. Styrene conversion was 95%.

[0027] Gas chromatography: column shape: SE-54; column temperature: 170°C; vaporization chamber: 240°C; detection chamber: 260°C; column front pressure: 0.08MPA.

Embodiment 2

[0029] In a 1000ml reaction bottle, put 150g of styrene and 450g of hydrochloric acid with a mass concentration of 25%, and stir and react at a temperature of 34-36°C for 10 hours, then stand for separation, wash the oil layer with water, dry and weigh 151.6g, α-chlorine The ethylbenzene content is 98.4%. Styrene conversion was 92%.

[0030] Gas chromatography: column shape: SE-54; column temperature: 170°C; vaporization chamber: 240°C; detection chamber: 260°C; column front pressure: 0.08MPA.

Embodiment 3

[0032] In a 500ml reaction bottle, put 100g of styrene and 400g of hydrochloric acid with a concentration of 30% at a temperature of 35-37°C, stir and react for 8 hours, then stand for stratification, wash the oil layer with water, finely separate the layers, and use sodium thiosulfate for the oil layer After drying for 2 hours, the concentration of the oil layer was weighed to be 97%, and the content of α-chloroethylbenzene analyzed by gas chromatography was 98%. Styrene conversion was 92%.

[0033] Gas chromatography: column shape: SE-54; column temperature: 170°C; vaporization chamber: 240°C; detection chamber: 260°C; column front pressure: 0.08MPA.

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Abstract

The invention discloses a preparation method of 2-phenylpropionic acid. The method comprises the following steps: stirring and reacting styrene and hydrochloric acid solution with the mass concentration of 20-30% used as raw materials for 8-14 hours at the temperature of 30-40 DEG C, standing and layering, water-washing an oil layer to obtain 2-chloro-ethylbenzene, and further sequentially performing cyanidation and hydrolysis on 2-chloro-ethylbenzene so as to prepare 2-phenylpropionic acid. The method adopts styrene as the raw material for direct chlorination, thereby reducing the reaction steps, being easy to control the conditions and being simple in equipment; and furthermore, the obtained product is stable in quality and high in purity, and the benefits are significantly improved.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a preparation method of 2-phenylpropionic acid. Background technique [0002] Existing 2-phenylpropionic acid products are usually prepared from acetophenone as a raw material by first reducing chlorine under high pressure hydrogenation and then by chlorination. The preparation steps of this method are complicated, the conditions are difficult to control and the cost is high. The present invention has carried out bold innovations, using styrene as a raw material, carried out a large number of experimental trial productions, and successfully used in industrialized production after being enlarged in a pilot test. In this process, styrene is used as raw material for direct chlorination, the number of reaction steps is reduced, the conditions are easy to control, and the obtained product has stable quality and high purity. Contents of the invention [0003] The objec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/30C07C51/08
Inventor 倪国成李剑平
Owner CHANGZHOU TIANHUA PHARMA
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