反应详情

A 250-mL round-bottomed flask was charged with [9-(2,5-dichlorobenzyl)-9H-β-carbolin-3-yl]methanol (1.84 g, 5.1 mmol), manganese (IV) oxide (1.14 g, 13.1 mmol) and dichloromethane (60 mL). The reaction mixture was stirred at room temperature for 12 hours. The mixture was filtered, concentrated in vacuo, and the residue chromatographed (hexane:ethyl acetate=10:1), affording the title compound (1.6 g, 87% yield). 1H NMR (CDCl3) δ10.3 (s, 1H), 8.9 (s, 1H), 8.8 (s, 1H), 8.3 (d,1H), 7.7 (t, 1H), 7.5-7.4 (m, 3H), 7.2 (s, 1H), 6.6 (s, 1H), 5.7 (s, 2H), MS (Cl); 355, 357, 359.

1. filtrationThe mixture was filtered
2. concentrationconcentrated in vacuo
3. customthe residue chromatographed (hexane:ethyl acetate=10:1)