反应详情

A mixture of indoline (D13, 0.30 g, 1.49 mmol), phenylcarbamate (D3, 0.48 g, 1.5 mmol) and triethylamine (0.20 ml, 1.5 mmol) in dry acetonitrile (10 mL) was warmed briefly to ensure complete solution of reactants, then stirred overnight at room temperature. The mixture was poured into water (50 ml) and the precipitate was filtered off, washed with water and dried. The crude product was chromatographed on silica gel (25 g) eluted with 4% methanol/dichloromethane. Eluted product was recrystallised from dichloromethane/methanol to give the title compound (0.35 g, 55%), m.p. 219-20° C.

1. temperaturewas warmed briefly
2. filtrationthe precipitate was filtered off
3. washwashed with water
4. customdried
5. customThe crude product was chromatographed on silica gel (25 g)
6. washeluted with 4% methanol/dichloromethane
7. customEluted product was recrystallised from dichloromethane/methanol