反应详情

5-Benzyloxy-2-(4-benzyloxyphenyl)isoindoline (400 mg) in TFA (12 mL) was refluxed under nitrogen atmosphere for 1 h and cooled. The solvents were removed under vacuum. The residue was dissolved in ethyl acetate (100 mL) and washed with saturated sodium bicarbonate (twice) then brine. Purification by chromatography on silica gel (eluant: dichloromethane—methanol 95:5) gave the title compound (95 mg) as a tan solid. 1H NMR (DMSO-d6): 9.35 (s, 1H), 8.53 (s, 1H), 7.14 (d, 1H, J=8.4 Hz), 6.75 (s br, 1H), 6.69 (m, 3H), 6.49 (d, 2H, J=8.7 Hz), 4.38 (m, 4H); MS: 228 (MH+).

1. temperaturecooled
2. customThe solvents were removed under vacuum
3. dissolutionThe residue was dissolved in ethyl acetate (100 mL)
4. washwashed with saturated sodium bicarbonate (twice) then brine
5. customPurification by chromatography on silica gel (eluant: dichloromethane—methanol 95:5)