Reaktion #3395

ord-b9f158cd252c4dcaaab2ab046391e1e9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed
  2. 2
    Sonstigethe precipitate was triturated with

Vorschrift

7a-(5-fluoro-3-pyridinyl)-hexahydro-1H-pyrrolizine (62 mg, 0.24 mmol, from step 12d) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with to give a white solid (57.1 mg, 69%). mp 168°-169° C. 1H NMR D2O, 300 MHz) 67 2.13-2.50 (m, 6H), 2.58-2.67 (m, 2H), 3.34-3.42 (m, 2H), 3.78-3.87 (m, 2H), 7.24 (dd, J=8.8, 2.4, Hz, 1H), 8.13 (ddd, J=8.8, 7.2, 2.7 Hz, 1H), 8.36 (dd, J=2.7, 1.4 Hz, 1H); MS (CI/NH3) m/z: 207 (M+H)+. Anal. Calcd for Cl12H16 ClFN2 : C, 59.38; H, 6.64; N, 11.54. Found: C, 59.51; H, 6.52; N, 11.30.

Quelle

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