Preparation method of alpha, beta-unsaturated ketone
An unsaturated, acetone-based technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemical methods, etc., can solve solid strong alkaline waste that is difficult to handle, does not conform to the spirit of green chemistry, and restricts large-scale production applications, etc. problems, to achieve the effect of simple synthesis method, high yield and mild reaction conditions
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Embodiment 1
[0012] In a 15mL high-pressure sealed tube, add immobilized proline and 2,6-dimethylpiperazine, dissolve benzaldehyde in 1 mL of acetone, and add this mixed solution into the high-pressure sealed tube under nitrogen protection at 50 Under the condition of ℃, stir for 48 hours (the feeding amount is shown in Table 1), the reaction solution gradually turns light yellow. After the reaction, petroleum ether was added to the reaction solution until no precipitate was precipitated, filtered, washed with petroleum ether, and dried to obtain a solid catalyst for next use. The filtrate was separated and purified by thin-layer chromatography (developing solvent: petroleum ether and ethyl acetate mixed at a volume ratio of 10:1) or purified by column chromatography to obtain the final product - ɑ, β-unsaturated ketone, with a yield of 81.2% .
[0013] substance molecular weight millimoles Mass / g Benzaldehyde 106 1 0.1060 acetone 58 3 0.1740 Immobilize...
Embodiment 2
[0016] Embodiment 2: other conditions are the same as embodiment 1, and the reaction is checked under different temperatures, and the experimental results are shown in Table 2.
[0017] serial number temperature(℃) Yield 1 20 46.6 2 30 53.8 3 40 64.5 4 50 81.2 5 60 76.1
[0018] It can be seen from the above table that the reaction temperature is the best under the condition of 50° C., and the yield is the highest.
Embodiment 3
[0019] Embodiment 3: other conditions are the same as embodiment 1, and the reaction under different co-catalyst conditions is checked, and the experimental results are shown in Table 3.
[0020] Table 3: Comparison table of the influence of different cocatalysts on the reaction
[0021]
[0022] It can be seen from the above table that the effect of using 2,6-dimethylpiperazine as the cocatalyst is the best, and the yield is the highest.
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