Reaktion #3408

ord-024cc166a8ad4750aa817d400f40ba7a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed
  2. 2
    Sonstigethe solid was dried

Vorschrift

7a-(3-Hydroxy-5-pyridinyl)-hexahydro-1H-pyrrolizine (150 mg, 0.56 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 dried to afford the title compound as a white powder (114 mg, 91%): mp 175°-180° C. (dec.); 1H NMR D2O, 300 MHz) δ2.11-2.63 (m, 8H), 3.35-3.44 (m, 2H), 3.80-3.89 (m, 2H), 7.66 (dd, J=2.4, 2.0 Hz, 1H), 8.23 (d, J=2.4 Hz, 1H), 8.29 (d, J=2.0 Hz, 1H); MS (CI/NH3) m/z: 205 (M+H)+. Anal. Calcd for C12H16N2O.HCl: C, 53.40; H, 6.65; N, 10.38. Found: C, 53.55; H, 6.62; N, 10.24.

Quelle

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