反应详情

To a solution of 2-(1-methylpiperidin-4-yloxy)-7-(piperidin-4-yloxy)-fluoren-9-one (81 mg, 0.21 mmol; Example 24A) in EtOAc (10 mL) containing a few drops of ethanol was added a solution of HCl in dioxane (4 M, 335 μL, 1.34 mmol; Aldrich). After stirring the mixture for 2 h, the solid was collected by filtration and recrystallized from hot EtOH-EtOAc to afford the title compound (50 mg, 0.11 mmol, 51% yield): 1H NMR (300 MHz, CD3OD) δ ppm 1.97-2.11 (m, 3H), 2.11-2.27 (m, 4H), 2.92 (s, 3H), 3.18-3.30 (m, 4H), 3.35-3.47 (m, 4H), 4.72-4.81 (m, 2H), 7.14 (dd, J=8, 2 Hz, 2H), 7.22 (d, J=2 Hz, 2H), 7.50 (d, J=8 Hz, 2H); MS (DCI/NH3) m/z 393 (M+H)+; Anal. C24H28N2O3.2HCl: C, H, N.

1. filtrationthe solid was collected by filtration
2. customrecrystallized from hot EtOH-EtOAc