反应详情

7a-(5,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 8b, 128 mg, 0.50 mmol) was slurried in Et2O (8 mL), and Et2O saturated with HCl (g) added. The solvent was removed, and the solid was recrystallized from MeOH/Et2O to afford a white solid (111 mg, 75%). mp 215°-217° C. MS (CI/NH3) m/e: 257 (M+H)+. 1H NMR D2O, 300 MHz) δ2.12-2.50 (m, 6H), 2.54-2.65 (m, 2H), 3.35-3.43 (m, 2H), 3.79-3.88 (m, 2H), 8.21 (d, J=2.4 Hz, 1H), 8.47 (d, J=2.4 Hz, 1H). Anal. Calcd for C12H15C13N2 : C, 49.09; H, 5.15; N, 9.54. Found: C, 49.01; H, 5.15; N, 9.44.

1. customThe solvent was removed
2. customthe solid was recrystallized from MeOH/Et2O