反应详情

温度

65 °C

A solution of 1-benzyl-4-(benzyloxy)-3-iodopyridin-2(1H)-one (1.9 g, 4.56 mmol) and vinyl-tri-butyltin (2.5 mL) in acetonitrile (20 0 mL) containing DMF (2.0 mL) was degassed using house vacuum and purged with argon. Then added PdCl2(PPh3)2 (0.3 g) and the mixture was heated at 65° C. under argon atmosphere for 4 h, with stirring. The solvents were distilled in vacuo, and the residue was triturated with EtOAc and filtered through a pad of celite. The filtrate was concentrated and the residue was purified by silica gel flash chromatography using 25% EtOAc in hexanes to give the title compound (0.75 g. 50%) as an orange colored solid.

1. customwas degassed
2. custompurged with argon
3. distillationThe solvents were distilled in vacuo
4. customthe residue was triturated with EtOAc
5. filtrationfiltered through a pad of celite
6. concentrationThe filtrate was concentrated
7. customthe residue was purified by silica gel flash chromatography