Reaktion #3387

Reaktionsgleichung

HCl

7a-(5,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine

→

solid

Ausbeute 151.2%

7a-(5,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine hydrochloride salt

Ausbeute 151.2%

Lösungsmittel

Et2O

Et2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed
2. 2
   Sonstigethe solid was recrystallized from MeOH/Et2O

Vorschrift

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.

Quelle