反应详情

A solution of precocene I (5.0 g, 26.3 mmol) in EtOH (200 mL) was hydrogenated by using 10% Pd/C (0.5 g) as catalyst. The catalyst was filtered of and EtOH was removed under reduced pressure. The crude material was then washed with dichloromethane (2×50 mL) to afford the desired product as white solid (4.55 g, 90%). 1H-NMR (CD3CN) δ 6.97 (d, J=8.0 Hz, 1H), 6.42 (d, J=8.0 Hz, 1H), 6.27 (s, 1H), 3.74 (s, 3 H), 2.72 (t, 2 H), 1.80 (t, 2 H), 1.32 (s, 6 H); MS LC-MS (MH+=193).

1. filtrationThe catalyst was filtered of and EtOH
2. customwas removed under reduced pressure
3. washThe crude material was then washed with dichloromethane (2×50 mL)