Reaktion #3410

ord-a1d18582f0384a23a908dc1e462f1ea7

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-(5-bromo-3-pyridinyl)-hexahydro-1H-pyrrolizine (107 mg, 0.52 mmol, from step 16c) was dissolved in methylene chloride, 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 an off-white powder (118 mg). mp 192°-194° C. 1H NMR D2O, 300 MHz) δ2.13-2.51 (m, 6H), 2.57-2.66 (m, 2H), 3.36-3.44 (m, 2H), 3.81-3.89(m, 2H), 8.22 (s, 1H), 8.65 (s, 1H), 8.72 (s, 1H); MS (CI/NH3) m/z: 267/269 (M+H)+. Anal. Calcd for C12 H15BrN2.HCl: C, 47.47; H, 5.31; N, 9.23. Found: C, 47.40; H, 5.22; N, 8.98.

Quelle

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