Method for synthesizing piperonal

A technology of jasmonal and oxygen, applied in the direction of organic chemistry, can solve the problems of nitrogen oxide pollution gas, complicated operation, large consumption of nitric acid, etc., and achieve the effect of reducing cost and simple operation

Inactive Publication Date: 2010-07-14
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above process has the following deficiencies: (1) the consumption of nitric acid is relatively large, and about every mole of 3,4-methylenedioxymandelic acid requires 0.65 to 1.00 moles of nitric acid; A large number of nitrogen oxides pollute the gas; (3) the operation is complicated, and the concentration of nitric acid or the drip rate of concentrated nitric acid needs to be strictly controlled

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Press 3,4-methylenedioxymandelic acid: nitric acid: sulfuric acid: the mol ratio of sodium nitrite is 1: 0.45: 1.00: 0.05, and the water addition is to make the concentration of nitric acid be 0.24mol / L as the criterion, and 3 , 4-methylenedioxymandelic acid, nitric acid, sulfuric acid, sodium nitrite and water are added to the reaction kettle at one time. Then, according to the molar ratio of 3,4-methylenedioxymandelic acid and oxygen as 1:0.5, oxygen was introduced, and the reaction vessel was sealed. Start stirring, and heat the reaction solution to 58°C. After 1.0 hours of reaction, cool the reaction solution to room temperature to obtain gas, liquid and solid, and separate the liquid and solid to obtain acidic filtrate and jasmonal products. The carbon dioxide in the gas product Recycled gas (containing nitrogen oxides and oxygen) is obtained after separation. The acidic filtrate and jasmonal product obtained by the reaction were analyzed by HPLC, and the yield of...

Embodiment 2

[0020] According to 3,4-methylenedioxymandelic acid: the molar ratio of nitric acid is 1:1.50, and the concentration of nitric acid is 1.00mol / L, add 3,4-methylenedioxymandelic acid and nitric acid solution at one time Reactor. Then, according to the molar ratio of 3,4-methylenedioxymandelic acid and oxygen as 1:0.01, oxygen was introduced, and the reaction vessel was sealed. Start stirring, and heat the reaction solution to 58°C. After reacting for 0.8h, cool the reaction solution to room temperature to obtain gas, liquid and solid, and separate the liquid and solid to obtain the acidic filtrate and jasmonal product. The carbon dioxide in the gas product Recycled gas (containing nitrogen oxides and oxygen) is obtained after separation. The acidic filtrate and jasmonal product obtained by the reaction were analyzed by HPLC, and the yield of jasmonal was 85.8%, and the reaction selectivity was 87.2%.

[0021] By 3, the mol ratio of 4-methylenedioxymandelic acid, nitrogen oxid...

Embodiment 3

[0024] Press 3,4-methylenedioxymandelic acid: nitric acid: sulfuric acid: the mol ratio of sodium nitrite is 1: 0.01: 3.00: 0.20, and the water addition is to make the nitric acid concentration be 0.05mol / L as the criterion, and 3 , 4-methylenedioxymandelic acid, nitric acid, sulfuric acid, sodium nitrite and water are added to the reaction kettle at one time. Then, according to the molar ratio of 3,4-methylenedioxymandelic acid and oxygen as 1:3.0, oxygen was introduced, and the reaction vessel was sealed. Start stirring, and heat the reaction solution to 30°C. After 24.0 hours of reaction, cool the reaction solution to room temperature to obtain gas, liquid and solid, and separate the liquid and solid to obtain acidic filtrate and jasmonal products. The carbon dioxide in the gas product Recycled gas (containing nitrogen oxides and oxygen) is obtained after separation. The acidic filtrate and jasmonal product obtained by the reaction were analyzed by HPLC, and the yield of j...

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Abstract

The invention relates to a method for synthesizing piperonal, which comprises the following steps of: adding 3,4-methylenedioxy benzene acid, nitric acid, sulfate, sodium nitrite and water into a reaction kettle by one step; after introducing oxygen gas, sealing the reaction kettle and obtaining acid filtrate, a piperonal product and recovered gas comprising nitrogen oxide and the oxygen gas after reacting; introducing the oxygen gas and the obtained recovered gas comprising the nitrogen oxide and the oxygen gas into the reaction kettle filled with the 3,4-methylenedioxy benzene acid and the acid filtrate, sealing the reaction kettle and obtaining the acid filtrate, the piperonal product and the recovered gas comprising the nitrogen oxide and the oxygen gas after reacting; and carrying out the operation repeatedly. The invention has the advantages of low cost, no pollution and simple operation.

Description

technical field [0001] The invention relates to a method for synthesizing jasmonal by using 3,4-methylenedioxymandelic acid as a raw material. Background technique [0002] Jasmonal is an important fine chemical, widely used in spices, medicine, pesticides, electroplating and other fields. [0003] The process of oxidative decarboxylation of 3,4-methylenedioxymandelic acid solid with nitric acid to prepare jasmonal is well known. At present, the known implementation process is as follows: after mixing about 2.6mmol mass fraction of 3.1% nitric acid and about 2.6mmol 3,4-methylenedioxymandelic acid, the product is dark oily liquid, and when the nitric acid mass fraction When the fraction is slightly reduced to 2.3%, the reaction hardly proceeds; about 1.177mol of concentrated nitric acid is added dropwise to about 1.5mol of 3,4-methylenedioxymandelic acid and hydrochloric acid, sodium nitrite, a small amount of nitric acid, water Under the protection of inert gas, 0.15mol c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/54
Inventor 高志贤郗宏娟王建国张素红庆绍军邱诗铭董凌曜胡蕴青
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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