反应详情

7a-(6-Chloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 5a, 210 mg, 0.94 mmol) was dissolved in Et2O (8 mL), and Et2O saturated with HCl (g) was added at ambient temperature. Solvent was then removed, and the remaining solid was recrystallized from MeOH/Et2O to afford short white needles (189 mg, 78%). mp 141°-143° C. MS (CI/NH3) m/e: 223 (M+H)+. 1H NMR D2O, 300 MHz) δ2.12-2.50 (m, 6H), 2.58-2.65 (m, 2H), 3.33-3.42 (m, 2H), 3.69-3.88 (m, 2H), 7.62 (d, J=8.5 Hz, 1HO, 7.99 (dd, J=8.5, 2.7 Hz, 1H), 8.53 (d, J=2.7 Hz, 1H). Anal. Calcd for C12H16Cl2N2 : C, 55.61; H, 6.22; N, 10.81. Found: C, 55.10; H, 6.36; N, 10.57.

1. customSolvent was then removed
2. customthe remaining solid was recrystallized from MeOH/Et2O