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Synthesis method for trans-3-hexenoic acid

A synthesis method and hexenoic acid technology are applied in chemical instruments and methods, carboxylate preparation, and ozone oxidation to prepare carboxylic acid, etc., which can solve the problems that the preparation method cannot meet the requirements, use, etc. Solvent residue, mild reaction effect

Inactive Publication Date: 2012-12-26
TIANNING FLAVOR JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The new food safety law stipulates that benzene and toluene cannot be used in edible flavors and fragrances. Therefore, the original preparation method of trans-3-hexenoic acid can no longer meet the requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of synthetic method of trans-3-hexenoic acid, carries out following steps successively:

[0020] 1) Prepare the mixed solution: add 60 parts of triethanolamine and 80 parts of malonic acid into a 250mL beaker, mix well;

[0021] 2) Dropping reaction: Add 300 parts of butyraldehyde into a 1000mL 4-neck round bottom flask, fill it with N 2 , heated to 80°C, stirring and dropping the mixed solution into butyraldehyde, the water generated by the reaction and butyraldehyde are azeotropic, the gas is condensed through the condenser tube, and the water generated by the reaction is collected, separated and removed in the oil-water separator until the oil-water separator is visually inspected There is no obvious water drop generation in the reaction system, and the content of malonic acid in the GC analysis reaction system is less than 0.1%, and the reaction stage lasts for 3.5 hours;

[0022] 3) Fractional distillation: fractionate butyraldehyde under the condition of v...

Embodiment 2

[0024] A kind of synthetic method of trans-3-hexenoic acid, carries out following steps successively:

[0025] 1) Prepare the mixed solution: add 80 parts of triethanolamine and 120 parts of malonic acid into a 500mL beaker, mix well;

[0026] 2) Dropping reaction: Add 400 parts of butyraldehyde into a 2000mL 4-neck round bottom flask, fill it with N 2 , heated to 60°C, stirred and added dropwise the mixed solution to butyraldehyde, the water generated by the reaction azeotropes with butyraldehyde, the gas is condensed through the condenser tube, and the water generated by the reaction is collected and separated in the oil-water separator until the oil-water separator is visually inspected There is no obvious water drop generation in the reaction system, and the content of malonic acid in the GC analysis reaction system is less than 0.1%, and the reaction stage lasts for 4 hours;

[0027] 3) Fractional distillation: fractionate butyraldehyde under the condition of vacuum 0.07...

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Abstract

The invention discloses a synthesis method for trans-3-hexenoic acid. According to the synthesis method, butyl aldehyde and malonic acid are used as starting raw materials, and triethanolamine is used as a catalyst. The synthesis method comprises the following steps of: preparing mixed solution, i.e., uniformly mixing and stirring the triethanolamine and the malonic acid according to the proportion of 1:3-3:1; performing dropping reaction, i.e., stirring and dropwise adding the mixed solution into the butyl aldehyde, charging N2 to protect the butyl aldehyde, heating to 60-100 DEG C, and separating by using an oil-water separator to remove water produced by the reaction, wherein the reaction time is 2-4 hours; and fractionating, i.e., removing the butyl aldehyde and front cut fraction through fractionation and then evaporating out a finished product. The trans-3-hexenoic acid synthesized by using the method has the characteristics of less isomer, mild reaction, simple process, high yield and no solvent residue.

Description

[0001] technical field [0002] The invention relates to a synthesis method of trans-3-hexenoic acid. Background technique [0003] Trans-3-Hexenoic Acid (trans-3-Hexenoic Acid) has a sweet berry aroma with a long-lasting smell, and is generally considered suitable for the deployment of food flavors. In the conventional preparation method of trans-3-hexenoic acid, the reaction solvent is benzene or toluene, and water is carried by benzene or toluene. The new food safety law stipulates that benzene and toluene cannot be used in edible flavors and fragrances. Therefore, the original preparation method of trans-3-hexenoic acid can no longer meet the requirements. Contents of the invention [0004] The object of the present invention is to provide a synthetic method of trans-3-hexenoic acid, which has simple process, high yield and no solvent residue. [0005] The purpose of the present invention is achieved through the following technical solutions: [0006] A synthetic me...

Claims

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Application Information

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IPC IPC(8): C07C57/03C07C51/38C07C51/353
Inventor 陈宗汉张树林周春飞
Owner TIANNING FLAVOR JIANGSU
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