反应详情

温度

80 °C

A 500 mL round bottom flask was charged with 77.E (21.5 g, 101 mmol), MeOH (300 mL), and sulfuric acid (1.08 mL, 20.3 mmol). The solution was stirred for 1 hour at 80° C., cooled to room temperature, and diluted with ether. The organic layers were washed with saturated aqueous NaHCO3, water, and brine, dried (MgSO4), and concentrated. The crude product was purified by silica gel flash chromatography (0-30% EtOAc/hexane) to afford 77.F (20.6 g, 90% yield) as a yellow oil.

1. temperaturecooled to room temperature
2. washThe organic layers were washed with saturated aqueous NaHCO3, water, and brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customThe crude product was purified by silica gel flash chromatography (0-30% EtOAc/hexane)