反应详情

温度

70 °C

To a mixture composed of ethyl 2-(2H-pyran-4(3H,5H,6H)-ylidene)acetate (10 g, 58.75 mmol) and ammonium formate (37 g, 587.54 mmol) in methanol (150 ml) was added 10% Pd-carbon (1.0 g) at room temperature, and the mixture was stirred at 70° C. for 15 hr. The reaction mixture was allowed to cool to room temperature, and the catalyst was collected by filtration through Celite pad and was washed with methanol. The filtrate was concentrated under reduced pressure, and the residue was chromatographed on silica gel column (hexane:ethyl acetate=94:6) to give the title compound as an oil (7.9 g, yield 78%).

1. temperatureto cool to room temperature
2. filtrationthe catalyst was collected by filtration through Celite pad
3. washwas washed with methanol
4. concentrationThe filtrate was concentrated under reduced pressure
5. customthe residue was chromatographed on silica gel column (hexane:ethyl acetate=94:6)