反应详情

2,3-Dichloropyridine (105.00 g, 710 mmol), Pd(OAc)2 (3.98 g, 17.74 mmol), rac-BINAP (16.57 g, 26.61 mmol), cesium carbonate (346.76 g, 1065 mmol), THF (1.05 L), and benzophenone imine (124.67 mL, 745 mmol) were added to a 2 L CHEMGLASS® Reactor fitted with a mechanical stirrer and reflux condenser. The mixture was heated to reflux with stirring for 18 h. The material was filtered, washed with THF (100 mL). The resulting filtrate was concentrated in vacuo to ⅓ volume and used without further purification. 1H NMR (CDCl3) δ 6.79 (dd, 1H, J=4.6, 7.6 Hz), 7.19-7.60 (m, 9H), 7.79-7.95 (m, 2H), 8.16 (dd, 1H, J=1.5, 5.1 Hz); MS (ESI+) m/z 293.1 (M+H)+.

1. customfitted with a mechanical stirrer
2. temperaturereflux condenser
3. temperatureThe mixture was heated
4. temperatureto reflux
5. filtrationThe material was filtered
6. washwashed with THF (100 mL)
7. concentrationThe resulting filtrate was concentrated in vacuo
8. customused without further purification