反应详情

温度

100 °C

A 100-mL round-bottomed flask equipped with a reflux condenser was charged with 151e (200 mg, 1.0 mmol), 3,5-dibromo-1-methylpyridin-2(1H)-one (268 mg, 1.0 mmol), Pd2(dba)3 (50 mg, 0.050 mmol), xantphos (58 mg, 0.10 mmol), Cs2CO3 (652 mg, 2.0 mmol) and 1,4-dioxane (20 mL). The system was subjected to three cycles of vacuum/argon flush and heated at 100° C. for 2 h. It was then cooled to room temperature and filtered. The solid was washed with dichloromethane (2×10 mL). The combined filtrate was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with dichloromethane/methanol (80:1 to 30:1) to afford 151f (300 mg, 79%) as a yellow solid. MS-ESI: [M+H]+ 380.2

1. customA 100-mL round-bottomed flask equipped with a reflux condenser
2. customflush
3. temperatureIt was then cooled to room temperature
4. filtrationfiltered
5. washThe solid was washed with dichloromethane (2×10 mL)
6. concentrationThe combined filtrate was concentrated under reduced pressure
7. customThe residue was purified by silica-gel column chromatography
8. washeluting with dichloromethane/methanol (80:1 to 30:1)