Industrial method for synthesizing 2-(4-methoxyphenoxy)-propionic acid through phase transfer

A technology of methoxyphenoxy and phase transfer catalysts, which is applied in the field of food science, can solve the problems of low product purity, high reaction temperature, and high production cost, and achieve the effects of shortening reaction time, improving conversion efficiency, and shortening reaction time

Active Publication Date: 2013-07-24
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method has high reaction temperature, long time, low yield and low product purity, so the production cost is high

Method used

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  • Industrial method for synthesizing 2-(4-methoxyphenoxy)-propionic acid through phase transfer
  • Industrial method for synthesizing 2-(4-methoxyphenoxy)-propionic acid through phase transfer
  • Industrial method for synthesizing 2-(4-methoxyphenoxy)-propionic acid through phase transfer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Add 10kg of p-hydroxyanisole, 11kg of sodium hydroxide, 0.4kg of phase transfer catalyst tetrabutylammonium bromide, and 150L of water into the reaction kettle, stir and mix at normal temperature and pressure, and the stirring speed is 150r / min. After reacting for 15 minutes, p-hydroxyanisole was converted into sodium p-methoxyphenate to obtain mixed material liquid A;

[0032] (2) Add 15kg of 2-chloropropionic acid and 150L of diethyl ether to the mixture liquid A, the reaction temperature is 40°C, the reaction pressure is 3MPa, the stirring speed is 150r / min, and the reaction is 1.5h to obtain the product 2-(4 -methoxyphenoxy)-propionic acid;

[0033] (3) After the reaction, the reaction solution is made acidic with 20% HCl solution, and the aqueous phase and the organic phase are separated by ether, and the 2-(4-methoxyphenoxy)-sodium propionate in the aqueous phase is transformed into 2-(4-methoxyphenoxy)-propionic acid enters the organic phase with diethyl eth...

Embodiment 2

[0036] (1) Add 10kg of p-hydroxyanisole, 20kg of sodium hydroxide, 0.6kg of phase transfer catalyst cyclodextrin, and 200L of water into the reaction kettle, stir and mix at normal temperature and pressure, the stirring speed is 200r / min, and react for 10min. Convert p-hydroxyanisole to sodium p-methoxyphenate to obtain mixed material liquid A;

[0037] (2) Add 15kg of 2-chloropropionic acid and 200L of n-hexane to the mixture liquid A, raise the reaction temperature to 45°C, the pressure is 2MPa, the stirring speed is 200r / min, and react for 1h to obtain the product 2-(4 -methoxyphenoxy)-propionic acid;

[0038] (3) After the reaction, the reaction solution was treated with 15% H 2 SO 4The solution is adjusted to be acidic, and the aqueous phase and the organic phase are separated by n-hexane, and the 2-(4-methoxyphenoxy)-sodium propionate in the aqueous phase is converted into 2-(4-methoxyphenoxy )-propionic acid enters the organic phase, and the organic phase is separate...

Embodiment 3

[0041] (1) Add 10kg of p-hydroxyanisole, 25kg of sodium hydroxide, 0.8kg of phase transfer catalyst cyclodextrin, and 150L of water into the reaction kettle, stir and mix at normal temperature and pressure, the stirring speed is 200r / min, and react for 10min. Convert p-hydroxyanisole to sodium p-methoxyphenate to obtain mixed material liquid A;

[0042] (2) Add 20kg of 2-chloropropionic acid and 160L of petroleum ether to the mixture liquid A, raise the reaction temperature to 40°C, the pressure is 2MPa, the stirring speed is 200r / min, and react for 1h to obtain the product 2-(4 -methoxyphenoxy)-propionic acid;

[0043] (3) After the reaction, the reaction solution was treated with 10% H 2 SO 4 The solution is adjusted to be acidic, and the aqueous phase and the organic phase are separated by petroleum ether, and the 2-(4-methoxyphenoxy)-sodium propionate in the aqueous phase is converted into 2-(4-methoxyphenoxy )-propionic acid enters the organic phase, and the organic ph...

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Abstract

The invention discloses an industrial method for synthesizing 2-(4-methoxyphenoxy)-propionic acid through phase transfer, which comprises the following steps of: stirring and mixing 4-Methoxyphenol, sodium hydroxide, a phase transfer catalyst and water, and reacting at normal temperature and normal pressure for 10 to 20 minutes to obtain mixed feed liquid; adding 2-chloro-propanoic acid and an organic phase into the mixed feed liquid, and reacting for 0.5 to 1.5 hours to obtain a product of 2-(4-methoxyphenoxy)-propionic acid; regulating the reaction liquid subjected to reaction to be acid byusing HCl or sulfuric acid solution, and standing to separate a water phase and the organic phase; and evaporating organic phase separation liquid to remove a solvent, and performing acid-base recrystallization to obtain the 2-(4-methoxyphenoxy)-propionic acid. When the reaction is finished, the yield of the 2-(4-methoxyphenoxy)-propionic acid is over 90 percent, the reaction temperature is reduced to 40-60 DEG C, the reaction time is only 0.5 to 1.5 hours, and the content of 2-(4-methoxyphenoxy)-propionic acid in the final product is 99.5 percent.

Description

technical field [0001] The invention belongs to the field of food science, and in particular relates to a new method for industrially preparing 2-(4-methoxyphenoxy)-propionic acid by using a phase transfer method. Background technique [0002] Sweetness inhibitors are a new class of additives that control or reduce the sweetness of sugary foods by blocking the receptors of sweetness and taste. Many traditional foods in China, such as candied fruit, moon cakes, chocolate, etc., use sucrose as a preservative. While achieving preservation, there is a problem of oversweetness to varying degrees. After using the sweetness inhibitor, it can not only play the functions of antisepsis and texture improvement of sucrose, but also not make the food too sweet and affect the taste. Therefore, the application prospect of sweetness inhibitor is very broad. [0003] Chinese invention patent ZL200510101321.1 has reported an industrial production method of a natural sweetness inhibitor trit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/68C07C51/367
Inventor 郑建仙葛亚中
Owner SOUTH CHINA UNIV OF TECH
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