Reaktion #44498

ord-4caae9e1348f4abdab29fcccbc4f0030

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was then evaporated
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in dichloromethane
  3. 3
    Waschenwashed with water, NaHCO3 solution, and brine
  4. 4
    Trocknenand dried (Na2SO4)
  5. 5
    FiltrationAfter filtration and evaporation of the solvent
  6. 6
    Sonstigethe amine was used without further purification

Vorschrift

The product of Example 7A (2.03 g, 10.38 mmol) was stirred at room temperature in the presence of ammonium acetate (8 g, 103.8 mmol) and NaBH3CN (3.3 g, 51.9 mmol) in methanol (30 mL) for twelve hours at 23° C. The solvent was then evaporated and the residue was dissolved in dichloromethane; washed with water, NaHCO3 solution, and brine; and dried (Na2SO4). After filtration and evaporation of the solvent, the amine was used without further purification.

Quelle

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