Reaktion #168152

ord-65afd247dabf40c0bf07b38d05555a76

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe resulting solution was washed with water and brine
  2. 2
    Trocknendried (Na2SO4)
  3. 3
    SonstigeAfter removal of the solvent
  4. 4
    Sonstigethe residue was purified by chromatography on silica gel (CH2Cl2/MeOH 99:1→90:10)

Vorschrift

Triethylamine (0.10 mL) and methyl chloroformate (24 μL) were added consecutively to (S)-6-(2-hydroxy-2-methyl-propyl)-6-phenyl-3-[(S)-1-(4-piperidin-4-yl-phenyl)-ethyl]-[1,3]oxazinan-2-one (0.12 g) dissolved in dichloromethane (5 mL) at room temperature. The resulting solution was stirred at room temperature overnight and then diluted with dichloromethane. The resulting solution was washed with water and brine and dried (Na2SO4). After removal of the solvent, the residue was purified by chromatography on silica gel (CH2Cl2/MeOH 99:1→90:10) to afford the title compound as a foam-like solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846668B2uspto-grants-2014_09