反应详情

The product of Example 36A (100 mg, 0.23 mmol) was treated with HCl (Aldrich, 4 M in dioxane, 2 mL, 8 mmol) in EtOH (5 mL) at ambient temperature for 1 h. The mixture was concentrated and the title compound was purified by chromatography (SiO2, EtOAc:MeOH (v. 2% NH3.H2O), 50:50, Rf. 0.1) as white solid (50 mg, 64%). 1H NMR (500 MHz, MeOH-D4) δ 1.47-1.64 (m, 1 H), 1.65-1.78 (m, 1 H), 1.78-1.91 (m, 1 H), 1.96-2.16 (m, 1 H), 2.15-2.38 (m, 1 H), 2.73-3.05 (m, 5 H), 3.35-3.47 (m, 1 H), 4.96-5.28 (m, 1 H), 7.10 (d, J=8.8 Hz, 1 H), 7.68 (dd, J=8.8, 2.1 Hz, 1 H), 8.32 (d, J=2.1 Hz, 1 H), 8.79 (s, 2 H) ppm. MS (DCl/NH3): 342 (M+H)+.

1. concentrationThe mixture was concentrated
2. customthe title compound was purified by chromatography (SiO2, EtOAc:MeOH (v. 2% NH3.H2O), 50:50, Rf. 0.1) as white solid (50 mg, 64%)