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 (200 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