反应详情

To a stirred solution of 7 (3.8 g, 21 mmol) in 250 mL CH2Cl2, MnO2 (11 g, 126 mmol) was added. The reaction mixture was stirred overnight, filtered on Celite® and the solvent was distilled under reduced pressure. The crude product was purified by a silica gel column with 17% EtOAc/83% Hexane as eluents. The product was isolated as pale yellow oil (70% yield). 1H NMR (CDCl3) δ 7.286 (dd, 1H, Ar), 7.195 (ddd, 1H, Ar), 7.063 (d, 1H, Ar), 7.003 (ddd, 1H, Ar), 4.669 (s, 2H, —CH2—), 1.447 (s, 9H, —C(CH3)3). Mass Spec.=203.09 (M+H)++Na+.

1. filtrationfiltered on Celite®
2. distillationthe solvent was distilled under reduced pressure
3. customThe crude product was purified by a silica gel column with 17% EtOAc/83% Hexane as eluents