反应详情

7a-(3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 3a, 125 mg, 0.66 mmol) was dissolved in CH2Cl2 (15 mL) and Et2O saturated with HCl (g) was added dropwise. The solvent was removed, and the remaining solid was triturated with CH2Cl2 (2×) to afford a hygroscopic yellow solid (140 mg, 81%). MS (CI/NH3) m/e: 189 (M+H)+. 1H NMR (D2O, 300 MHz) δ2.13-2.29 (m, 2H), 2.32-2.43 (m, 2H), 2.48-2.69 (m, 4H), 3.40-3.49 (m, 2H), 3.83-3.92 (m, 2H), 7.92 (dd, J=8.5, 5.5 Hz, 1H), 8.43 (ddd, J=8.5, 2.6, 1.4 Hz, 1H), 8.75 (dd, J=5.5, 1.4 Hz, 1H), 8.88 (d, J=2.6 Hz, 1H). Anal. Calcd for C12H18Cl2N2.0.5H2O: C, 53.34; H, 7.09; N, 10.37. Found: C, 53.28; H, 6.96; N, 10.22.

1. customThe solvent was removed
2. customthe remaining solid was triturated with CH2Cl2 (2×)