反应详情

A mixture of 3-fluoro-5-iodoaniline (0.47 g, 1.98 mmol) and 1,1′-carbonyl imidazole (0.33 g, 2 mmol) in dichloromethane (40 ml) was stirred at room temperature for 1 h, then evaporated to dryness. To the residue was added dimethylformamide (DMF, 10 ml) and a solution of 5-methoxy-6-trifluoromethylindoline (D11, 0.44 g, 2 mmol) in DMF (5 ml). The mixture was heated at 80° C. overnight, then cooled and poured into water. The precipitate was filtered off, washed with water and dried. The crude product was chromatographed on silica gel and eluted with dichloromethane. Eluted product was recrystallised from dichloromethane to give the title compound (0.38 g, 40%), m.p. 221-4° C.

1. customevaporated to dryness
2. additionTo the residue was added dimethylformamide (DMF, 10 ml)
3. temperatureThe mixture was heated at 80° C. overnight
4. temperaturecooled
5. filtrationThe precipitate was filtered off
6. washwashed with water
7. customdried
8. customThe crude product was chromatographed on silica gel
9. washeluted with dichloromethane
10. customEluted product was recrystallised from dichloromethane