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Synthesis method of 2-hexenal

A synthetic method, the technology of hexenal, which is applied to the preparation of heterocyclic compounds, the separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of unsuitability for industrial production, many reaction steps, and cumbersome processes, etc., to prevent pollution, Simplify the steps and ensure the effect of high purity

Active Publication Date: 2017-02-08
HUBEI JINGHONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many reaction steps, complex process, low yield after multi-step reaction, and is not suitable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 0.03 equivalent boron trifluoride ethyl ether solution to the reaction bottle, add dropwise a mixture of 50 g vinyl ether and 110 g n-butyraldehyde, control the temperature at 30-35 °C, stir for 1 hour after the dropwise addition, and add 10% trichloro Add 204 grams of iron oxide aqueous solution into another reaction flask to raise the temperature, add the aforementioned reaction solution dropwise, and distill while adding dropwise. Add 0.2% by weight hydroquinone to the distilled crude product, first rectify the low boilers at atmospheric pressure, continue rectifying under reduced pressure, and collect 2 - Pure hexenal, yield 78%, GC: 99.4%.

Embodiment 2

[0018] Add 0.05 equivalent of boron trifluoride ether solution to the reaction bottle, dropwise add 50 g of vinyl ether and 133 g of n-butyraldehyde mixture, control the temperature at 25-40 ° C, stir for 1 hour after the addition is complete, and add 6% trichloro After adding 700 grams of iron oxide aqueous solution into another reaction flask, the temperature was raised, and the aforementioned reaction solution was added dropwise, and distilled while adding dropwise. Add 0.2% by weight hydroquinone to the distilled crude product, first rectify the low boilers at atmospheric pressure, continue rectifying under reduced pressure, and collect 2 - Pure hexenal, yield 82%, GC: 99.2%.

Embodiment 3

[0020] Add 0.03 equivalents of boron trifluoride ether solution to the reaction bottle, dropwise add a mixture of 100 g of vinyl ether and 250 g of n-butyraldehyde, control the temperature at 40-50 ° C, stir for 1 hour after the addition is complete, and 10% chlorinated Add 408 grams of zinc aqueous solution into another reaction flask and then heat up, add the aforementioned reaction solution dropwise, and distill while adding dropwise, add 0.3% by weight hydroquinone to the crude product distilled out, and first normal pressure rectification goes out the low boiler, Continuous rectification under reduced pressure, when the pressure is -0.09MPa, and the tower top temperature is 78-80°C, the pure product of 2-hexenal is collected, the yield is 80%, GC: 99.3%.

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Abstract

The invention discloses a synthesis method of 2-hexenal. The method includes: adding a mixed solution of n-butanal and vinyl alkyl ether into a catalyst boron trifluoride diethyl etherate solution dropwise to carry out reaction, subjecting the obtained acetal to heating hydrolysis distillation under the catalytic action of a Lewis acid aqueous solution, and subjecting an obtained 2-hexenal crude product to continuous pressure reduction distillation, thus obtaining high purity 2-hexenal. The method provided by the invention has the characteristics of stable route and process and high yield, and the product has competitive edge.

Description

technical field [0001] This description relates to a synthetic method of 2-hexenal, which belongs to the technical field of organic synthesis. Background technique [0002] 2-Hexenal has been widely used in the formulation of daily chemical flavors, mainly for the preparation of raspberry, mango, egg fruit, apple, strawberry and other flavors. This product has a fresh green leaf fragrance and can be used for artificial flowers and essential oils , All kinds of floral blend spices. [0003] The method in the prior art mainly adopts hexanal to react with ethylene glycol after bromination, and then hydrolyzes to obtain it. The method has many reaction steps, complicated process, low yield after multi-step reaction, and is not suitable for industrial production. Contents of the invention [0004] In order to overcome the deficiencies of the prior art, the present invention provides a scheme for obtaining high-purity 2-hexenal through continuous vacuum distillation after hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/60C07C45/86C07C47/21
CPCC07C45/60C07C45/86C07D319/06C07C47/21
Inventor 杨辉赵亚运朱美山华兴雷陈雷
Owner HUBEI JINGHONG CHEM
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