反应详情

To a solution of Example 1D (100 mg, 0.23 mmol) in dichloromethane (2 mL), was added hydrogen chloride-saturated ethyl acetate (2 mL) and the mixture was stirred at room temperature for 2 hours. The mixture was concentrated and purified by preparative HPLC (Agilent AD/SP/C18-25/011 reversed phase column) eluting with a gradient of 0.01% trifluoroacetic acid in water to 1:1 methanol/acetonitrile to afford the title compound as the hydrochloride salt. LCMS: 327.1 (M+H)+; 1H NMR (400 MHz, DMSO-d6/D2O): δ 1.77-1.87 (m, 2H), 2.23 (d, J=12 Hz, 2H), 3.0-3.06 (m, 2H), 3.33-3.41 (m, 3H), 3.79 (s, 3H), 6.45 (s, 1H), 7.29-7.32 (m, 1H), 7.44-7.50 (m, 2H), 8.99 (s, 1H).

1. concentrationThe mixture was concentrated
2. custompurified by preparative HPLC (Agilent AD/SP/C18-25/011 reversed phase column)
3. washeluting with a gradient of 0.01% trifluoroacetic acid in water to 1:1 methanol/acetonitrile