反应详情

To neat (S)-tert-butyl 4-methoxy-3,3-dimethylpiperidine-1-carboxylate (5.87 g, 24.1 mmol) was added 4.0 M HCl in dioxane (24.1 mL, 96.0 mmol), and the reaction mixture was stirred at room temperature for 16 h. Then, the reaction mixture was diluted with heptanes (60 mL) and Et2O (10 mL) and stirred at room temperature until a white solid crashed out. The heterogeneous mixture was then filtered and the white solid was collected to afford (S)-4-methoxy-3,3-dimethylpiperidin-1-ium chloride. 1H NMR (400 MHz, CDCl3) δ ppm 9.58 (br. s., 1 H), 9.23 (br. s., 1 H), 3.34 (s, 3 H), 3.09-3.24 (m, 2 H), 3.05 (t, J=10.0 Hz, 1 H), 2.97 (dd, J=5.4, 2.4 Hz, 1 H), 2.76 (d, J=13.1 Hz, 1 H), 2.04-2.17 (m, 1 H), 1.84-1.96 (m, 1 H), 1.19 (s, 3 H), 1.05 (s, 3 H).

1. stirringstirred at room temperature until a white solid
2. filtrationThe heterogeneous mixture was then filtered
3. customthe white solid was collected