反应详情

温度

70 °C

A slurry of Compound 4 (60 mg) and K2CO3 (43 mg) in deionized water (1 mL) was stirred at room temperature for 30 min. To the resulting reaction mixture, t-BuOH (1 mL) and pyrrolidine (52 μL) were added and heated at 70° C. for 5 hours. The reaction mixture was then concentrated under reduced pressure and the residue was dissolved in acetic acid (10 mL) and stirred at room temperature for 2 hours. The acetic acid solution was concentrated again under vacuum. Finally, the residue was partitioned between chloroform (2×15 mL) and 7% aqueous NaHCO3 solution (5 mL). The collective organic layers were dried, concentrated and purified on a silica gel using 10% ethanol in dichloromethane to afford the required product in 83% yield (45 mg).

1. additionwere added
2. concentrationThe reaction mixture was then concentrated under reduced pressure
3. dissolutionthe residue was dissolved in acetic acid (10 mL)
4. concentrationThe acetic acid solution was concentrated again under vacuum
5. customFinally, the residue was partitioned between chloroform (2×15 mL) and 7% aqueous NaHCO3 solution (5 mL)
6. customThe collective organic layers were dried
7. concentrationconcentrated
8. custompurified on a silica gel using 10% ethanol in dichloromethane