Method for efficiently synthesizing 1,6-diene-3-ketone derivatives
A technology of ketone derivatives and dienes, applied in the field of efficient synthesis of 1,6-dien-3-one derivatives, can solve the difficulties of 1,6-dien-3-one derivatives, harsh reaction conditions, pollution Environmental and other issues, to achieve the effect of novel structure, mild reaction conditions, and simple operation
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Embodiment 1
[0025] Embodiment 1: preparation compound 1a
[0026] Bis(triphenylphosphine)palladium dichloride (0.35g, 0.5mmol) and ketone iodide (0.19g, 1mmol) were added into a 500mL Shrek bottle, and the solvent triethylamine ( 200mL), iodobenzene (11.22g, 55mmol) and 4-pentynol (4.2g, 50mmol), react at room temperature for 12 hours. Extracted with ethyl acetate, dried over anhydrous magnesium sulfate, suction filtered, concentrated under reduced pressure in vacuo, the eluent was ethyl acetate:petroleum ether=1:3, separated by column chromatography to obtain 4-pentyn-1-ol (7.6g , 95%).
[0027] 4-Pentyn-1-ol (7.6g, 47.5mmol) was dissolved in dichloromethane (50mL) solvent, and Dess Martin (22.2g, 52.3mmol) oxidant solid particles were slowly added at 0°C, and the temperature was raised to room temperature to continue React for 2 hours. The solid was removed by suction filtration, the filtrate was quenched with saturated aqueous sodium bicarbonate, extracted with dichloromethane, drie...
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