反应详情

温度

0 °C

To a solution (100 mL) of tert-butyl diethylphosphonoacetate (13.8 g, 51.8 mmol) in tetrahydrofuran was added 60% sodium hydride (2.45 g, 61.2 mmol) with stirring at 0° C., and the mixture was stirred at the same temperature for 15 min. Then, to this mixture was added dropwise a solution (138 mL) of 4-(benzyloxy)benzaldehyde (10 g, 47.1 mmol) in tetrahydrofuran with stirring at 0° C., and the mixture was stirred at room temperature for 3 hrs. The reaction mixture was concentrated, and the residue was diluted with ethyl acetate, and washed with 5% aqueous potassium hydrogensulfate solution and saturated brine. The ethyl acetate layer was dried over magnesium sulfate, and concentrated under reduced pressure to give the title compound (13.7 g, yield 94%) as colorless crystals.

1. stirringthe mixture was stirred at the same temperature for 15 min
2. stirringwith stirring at 0° C.
3. stirringthe mixture was stirred at room temperature for 3 hrs
4. concentrationThe reaction mixture was concentrated
5. additionthe residue was diluted with ethyl acetate
6. washwashed with 5% aqueous potassium hydrogensulfate solution and saturated brine
7. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
8. concentrationconcentrated under reduced pressure