反应详情

A mixture of 174A (48.5 g, 0.178 mol) and palladium/carbon (4.6 g) in EtOAc (450 mL) was evacuated under reduced pressure and charged with hydrogen (3×). The reaction mixture was subsequently stirred under a steady stream of nitrogen for 1 h. The reaction mixture was filtered through a pad of Celite, concentrated, and recrystallized form a mixture of MeOH and DCM to provide 36.2 g (90%) of 174B as a bright yellow solid. HPLC retention time=2.68 min. (Condition B), and LC/MS M+1=228. 1H-NMR (500 MHz, CDCl3) δ 3.89 (s, 3H), 3.92 (s, 3H), 7.20 (d, 1H), and 7.61 (d, 1H).

1. customwas evacuated under reduced pressure
2. additioncharged with hydrogen (3×)
3. filtrationThe reaction mixture was filtered through a pad of Celite
4. concentrationconcentrated
5. customrecrystallized form
6. additiona mixture of MeOH and DCM