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

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

Active Publication Date: 2011-04-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method has high reaction temperature, long time, l

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

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Experimental program
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Effect test

Embodiment 1

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

[0032] (2) In the mixture liquid A, add 15kg of 2-chloropropionic acid, 150L of ether, 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) The reaction solution after the reaction is adjusted to be acidic with 20% HCl solution, and the water phase and the organic phase ether are separated by standing, and the 2-(4-methoxyphenoxy)-sodium propionate in the water phase is converted 2-(4-methoxyphenoxy)-propionic acid enters the organic phase with diethyl ether, and the organic phas...

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 respectively, 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) In the mixture liquid A, add 15kg of 2-chloropropionic acid, 200L of n-hexane, 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) The reaction solution after the reaction was treated with 15% H 2 SO 4The solution is adjusted to be acidic, and the aqueous phase and the organic phase n-hexane are separated by standing, and the 2-(4-methoxyphenoxy)-sodium propionate in the aqueous phase is converted into 2-(4-methoxyphenoxy )-propionic acid enters the organic phase, and separates ...

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

[0043] (3) The reaction solution after the reaction was treated with 10% H 2 SO 4 The solution is adjusted to be acidic, and the aqueous phase is separated from the organic phase 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, a...

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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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IPC IPC(8): C07C59/68C07C51/367
Inventor 郑建仙葛亚中
Owner SOUTH CHINA UNIV OF TECH
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