Reaktion #44508

ord-329e3ec9dae6413cb347606bd05c3108

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated
  2. 2
    Sonstigethe residue was partitioned with dichloromethane and water
  3. 3
    WaschenThe organic phase was washed with NaHCO3 solution and brine
  4. 4
    Trocknendried (Na2SO4)
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigeevaporated
  7. 7
    SonstigeThe crude title compound was used in the following step without further purification

Vorschrift

The product of Example 10B (0.259 g, 1.71 mmol), ammonium acetate (1.32 g, 17.14 mmol), and sodium cyanoborohydride (0.43 g, 6.84 mmol) was stirred in methanol (8 mL) for twelve hours. The solvent was evaporated and the residue was partitioned with dichloromethane and water. The organic phase was washed with NaHCO3 solution and brine, dried (Na2SO4), filtered, and evaporated. The crude title compound was used in the following step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737137B2uspto-grants-2010_06