反应详情

To a suspension of 8 (6.28 g, 20.0 mmol) in ethanol (200 mL) palladium on carbon (10%, wet, 0.63 g) was added and stirred under H2 at atmospheric pressure at room temperature for 18 h. Catalyst was filtered through a bed of Celite® and solvent was evaporated under reduced pressure to yield 15 as white solid (6.32 g, 100%): mp 63-65° C.; 1HNMR (400 MHz, DMSO-d6): δ 7.15 (d, J=8.7 Hz, 2H), 6.74 (d, J=8.7 Hz, 2H), 6.29 (t, J=2.4 Hz, 1H), 6.25 (d, J=2.4 Hz, 2H), 3.78 (t, J=8.7 Hz, 1H), 3.72 (s, 6H), 3.62 (s, 3H), 3.31 (dd, J=13.5 and 8.4 Hz, 1H), 2.93 (dd, J=13.5 and 6.9 Hz, 1H); MS (EI) m/z 317[M]+; Anal. (C18H20O5) C, H.

1. additionwas added
2. filtrationCatalyst was filtered through a bed of Celite® and solvent
3. customwas evaporated under reduced pressure