反应详情

To a solution of 2,7-bis-(1-methylpiperidin-4-yloxy)-fluoren-9-one (110 mg, 0.27 mmol; Example 24A) in ethyl acetate (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 (74 mg, 0.155 mmol, 57% yield): 1H NMR (300 MHz, CD3OD) δ ppm 1.93-2.36 (m, 8H), 2.92 (s, 6H), 3.10-3.29 (m, 4H), 3.32-3.51 (m, 4H), 4.57-4.78 (m, 2H), 7.10-7.29 (m, 4H), 7.50 (d, J=8 Hz, 2H); MS (DCI/NH3) m/z 407 (M+H)+; Anal. C25H30N2O3.2HCl 0.1H2O: C, H, N.

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