反应详情

HATU (0.38 g, 0.99 mmol), diisopropylethylamine (0.41 mL, 2.48 mmol) and morpholine (0.08 mL, 0.99 mmol) were added at 0° C. to a solution of 300b) (0.35, 0.83 mmol) in dry DMF (2 mL). The reaction mixture was stirred at room temperature for 6 h and then quenched with ice-cold water. The mixture was extracted with dichloromethane (2×50 mL), the combined organic layers were dried over sodium sulfate and the solvent was removed in vacuo. The remnant was purified by flash column chromatography [silica, dichloromethane with 1.5% methanol]. White solid. Yield: 0.32 g (80% of theory)

1. customquenched with ice-cold water
2. extractionThe mixture was extracted with dichloromethane (2×50 mL)
3. dry with materialthe combined organic layers were dried over sodium sulfate
4. customthe solvent was removed in vacuo
5. customThe remnant was purified by flash column chromatography [silica, dichloromethane with 1.5% methanol]