反应详情

To a stirred solution of 2-tributylstannyl-2,3-dihydropyran (Example 6, 0.41 g, 0.11 mmol) in anhydrous toluene (15 mL) was added 5-bromo-3-(N-methylpyrrolidin-3-yl)-1-benzoylindole (Example 5b, 0.280 g, 0.729 mmol) and Pd[PPh3 ]4 (0.09 g, 0.076 mmol). The mixture was heated to reflux for 6.5 hours, cooled, filtered through celite and concentrated by reduced pressure. The crude product was purified by column chromatography [95:5 CH2Cl2 : NH3 (2M in MeOH)] to yield the title compound (0.241 g, 85%) as a yellow oil; HRMS-FAB+ for C25H26N2O2 ; calc. MH+ :387.2072; found MH+ :387.2092.

1. temperatureThe mixture was heated
2. temperatureto reflux for 6.5 hours
3. temperaturecooled
4. filtrationfiltered through celite and
5. concentrationconcentrated by reduced pressure
6. customThe crude product was purified by column chromatography [95:5 CH2Cl2 : NH3 (2M in MeOH)]