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
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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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