反应详情

7-[3-(3-Bromo-2-oxo-2H-quinolin-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.5 g), phenylboronic acid (0.12 g), tetrakis(triphenyl phosphine)palladium (0) (0.11 g), and potassium carbonate (0.39 g) were added to dioxane (5 ml). The mixture was heated under reflux for 2 hours under nitrogen atmosphere. The reaction mixture was cooled to room temperature. Water was added thereto, followed by extraction by ethyl acetate. The organic layer was dried over sodium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→3:1). The purified product was condensed to dryness under reduced pressure, thereby obtaining the title compound (0.34 g) as a white amorphous solid.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 2 hours under nitrogen atmosphere
3. extractionfollowed by extraction by ethyl acetate
4. dry with materialThe organic layer was dried over sodium sulfate, and condensed under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→3:1)
6. customcondensed to dryness under reduced pressure