反应详情

Activated Raney-Ni (0.54 g) in DMF (10 mL) was added to a solution of Example 126k (0.73 g, 1.276 mmol) in DMF (25 mL) and the reaction mixture was subjected to hydrogenation at 30 psi for 2 h. It was filtered through celite, concentrated and purified using flash chromatography (silica gel, 1.5% methanol/chloroform) to obtain the title compound. Yield: 0.54 g, (75.5%); 1H NMR (CDCl3): δ 2.5 (t, 4H, 2CH2), 2.7 (s, 3H, CH3), 3.22 (t, 4H, 2CH2), 3.5 (s, 2H, CH2), 3.7 (bs, 2H, NH2), 3.9 (s, 3H, OCH3), 4.65 (s, 2H, CH2), 6.6 (d, 1H, Ar), 6.7 (s, 1H, Ar), 6.72 (d, 1H, Ar), 6.77 (s, 1H, Ar), 6.9 (s, 1H, Ar), 7.1 (t, 1H, Ar), 8.08 (s, 1H, Ar), 8.5 (s, 1H, Ar); MS: m/e (CI+) 542 (M+1).

1. filtrationIt was filtered through celite,
2. concentrationconcentrated
3. custompurified