反应详情

Slurry 6-bromo-nicotinonitrile (8.0 g, 43.7 mmol), 1-ethoxyvinyl-tributylstannane (17.4 g, 48 mmol), and dichlorobis(triphenylphosphine)-palladium (1.5 g, 2.2 mmol) in acetonitrile (680 mL) at room temperature. Stir the mixture at reflux for 16 h under a nitrogen atmosphere. Cool the mixture to room temperature, add aqueous saturated potassium fluoride (100 mL), stir 30 min then filter and wash with EtOAc (200 mL). Wash the organic phase with water (250 mL). Dry the organic layer over Na2SO4, filter and concentrate in vacuo to obtain the desired intermediate (14.5 g) that was used without further purification. MS (ES+) m/z: 175 (M+H)+.

1. customat room temperature
2. temperatureat reflux for 16 h under a nitrogen atmosphere
3. stirringstir 30 min
4. filtrationthen filter
5. washwash with EtOAc (200 mL)
6. washWash the organic phase with water (250 mL)
7. dry with materialDry the organic layer over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo