反应详情

温度

100 °C

A 100 mL round-bottomed flask equipped with a reflux condenser was charged with 6-aminopyridin-2-ol (1.1 g, 10.0 mmol), 3,5-dibromo-1-methylpyridin-2(1H)-one (2.67 g, 10.0 mmol), cesium carbonate (6.52 g, 20.0 mmol), xantphos (576 mg, 1.0 mmol), Pd2(dba)3 (460 mg, 0.50 mmol), and DMF (35 mL). The system was subject to three cycles of vacuum/argon flush and heated at 100° C. for 3 h. It was then cooled to room temperature and filtered. The filtrate was diluted with DCM (500 mL) and washed with H2O (80 mL×3). The organic layer was dried and concentrated under reduced pressure. The residue solid was purified by silica-gel column-chromatography eluting with DCM/MeOH (30:1 to 15:1) to afford 101a (580 mg, 20%) as yellow solid. MS-ESI: [M+H]+ 296.0

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. additionThe filtrate was diluted with DCM (500 mL)
6. washwashed with H2O (80 mL×3)
7. customThe organic layer was dried
8. concentrationconcentrated under reduced pressure
9. customThe residue solid was purified by silica-gel column-chromatography
10. washeluting with DCM/MeOH (30:1 to 15:1)