Reaktion #3416

ord-b41b8bae64dd42eb82a4b840e4ce0359

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed
  2. 2
    Sonstigethe solid was crystallized from MeOH/Et2O
  3. 3
    Sonstigedried

Vorschrift

7a-(6-Chloro-5-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine (245 mg, 1.03 mmol) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was crystallized from MeOH/Et2O and dried to afford the title compound as white plates: mp 179°-180° C.; 1H NMR D2O, 300 MHz) δ2.14-2.48 (m, 9H) 2.56-2.65 (m, 2H), 3.34-3.42 (m, 2H), 3.79-3.87 (m, 2H), 7.89 (d, J=3.0 Hz, 1H), 8.33 (d. J=3.0 Hz, 1H); MS (CI/NH3) m/z: 237/239 (M+H)+ ; MS (CI/NH3): m/z 237 (M+H+). Anal. Calcd for C13H17ClN2.HCl.0.2 HCl: C, 55.67; H, 6.54; N, 9.99. Found: C, 55.90; H, 6.57; N, 9.76.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05733912uspto-grants-1998_03