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Method for preparing piperic acid through phase-transfer catalytic oxidation of piperonal

A technology of phase-transfer catalysis and phase-transfer catalyst, applied in the direction of chemical recovery, etc., can solve the problems of limited application fields, inability to use, and low yield, and achieve the effects of convenient recycling, simple methods, and reduced reaction time

Inactive Publication Date: 2016-07-06
福建仁宏医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The classic method of synthesizing piperic acid is to use potassium permanganate as an oxidant to oxidize piperonal to synthesize piperic acid, but its yield is low and it is easy to produce many by-products. Since the material cannot be absolutely dry, the product contains a small amount of moisture, resulting in Contains many by-products, so that the application field of the product is limited, and it cannot be used in many occasions

Method used

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  • Method for preparing piperic acid through phase-transfer catalytic oxidation of piperonal
  • Method for preparing piperic acid through phase-transfer catalytic oxidation of piperonal
  • Method for preparing piperic acid through phase-transfer catalytic oxidation of piperonal

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Experimental program
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Effect test

Embodiment 1

[0033] In a 2L reaction flask, first add 125g of dichloroethane, then 30g of jasmonal and 3g of a phase transfer catalyst, the phase transfer catalyst is tetramethylammonium bromide, and add 300ml of deionized water after dissolving. Then add 3g of liquid caustic soda and 6g of potassium permanganate every 10 minutes, and add 30g of liquid caustic soda and 60g of potassium permanganate ten times in total. After adding all the liquid caustic soda and potassium permanganate, slowly raise the temperature to 40°C-45°C and continue the reaction for 3h. Take the dichloroethane phase clear liquid, inject sample analysis, the content of jasmonal is required to be less than 0.5, if not, continue to add a small amount of potassium permanganate, control the pH > 9 and react for half an hour, take a sample and detect the content of jasmonal is 0.5 the following. After the reaction, the temperature was lowered, filtered, static layered, dichloroethane was separated and extracted twice wit...

Embodiment 2-15

[0035] In embodiment 2-15, except changing jasmonal, deionized water, phase transfer catalyst, liquid caustic soda, potassium permanganate and reaction time, react similarly with embodiment 1, and specific formula is shown in table 1 for details, specific See Table 2 for the details of the process conditions, the amount of phase transfer catalyst and the product yield.

[0036] Table 1

[0037]

[0038]

[0039] Table 2

[0040]

[0041]

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Abstract

The invention discloses a method for preparing piperic acid through phase-transfer catalytic oxidation of piperonal.The method comprises the following reaction and treatment steps that 1, dichloroethane is added into a reaction flask with a stirring device, a reactant piperonal and a phase-transfer catalyst are added, and deionized water is added finally; 2, caustic soda liquid and potassium permanganate are each divided into 10 parts and added into the reaction flask in ten times respectively; 3, the quantity of residual piperonal is detected through a reaction to enable the quantity of residual piperonal to reach a preset value; 4, the product piperic acid is finally obtained after the treatment methods such as cooling, filtering, extracting and drying are conducted.According to the method, the phase-transfer catalyst is added, and the mode of adding caustic soda liquid and potassium permanganate is changed, so that the reaction time is shortened, and the yield of piperic acid is greatly increased and increased to 90% or above from original 50% or above.In addition, the phase-transfer catalyst can be recycled, and cyclic utilization of next time is convenient.

Description

technical field [0001] The invention relates to a method for preparing piperic acid through phase-transfer catalytic oxidation of jasmonal. Background technique [0002] Piperic acid is an important pharmaceutical intermediate. In many synthetic reactions, we often use this compound to introduce piperonyl. It is an important intermediate of antibacterial drugs ciloxacin, minoxacin, cardiovascular drug oxolinic acid, anticancer drugs and cardiotonic agents, and can also be used in the production of spices, dyes and special textiles. The classic method of synthesizing piperic acid is to use potassium permanganate as an oxidant to oxidize piperonal to synthesize piperic acid, but its yield is low and it is easy to produce many by-products. Since the material cannot be absolutely dry, the product contains a small amount of moisture, resulting in Containing many by-products, the application field of the product is limited to a certain extent, and it cannot be used in many occasi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/60
CPCY02P20/584C07D317/60
Inventor 樊彬王国洪刘志铭黄京波
Owner 福建仁宏医药化工有限公司