Reaktion #1446546

ord-c95f5afe59c04780b903f073cb3b87fb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe organic phase was washed with sodium thiosulfate, water and brine
  4. 4
    Sonstigethe solvent was removed
  5. 5
    Wascheneluted with hexane/ethyl acetate (5:1)

Vorschrift

708 mg of N-iodosuccinimide was added little by little to a mixture of 783 mg of 2-benzyl-6-(cis-3,4-dimethoxypyrrolidine-1-yl)pyridine and 7.0 ml of N,N-dimethylformamide under ice-cooling, followed by stirring overnight as it was. The reaction solution was poured into water and extracted with ethyl acetate. The organic phase was washed with sodium thiosulfate, water and brine, and the solvent was removed. Then, the residue was subjected to NH-silica gel (Fuji Silicia) column chromatography and eluted with hexane/ethyl acetate (5:1) and then with hexane/ethyl acetate (3:1), to give 995 mg of the target compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06599917B1uspto-grants-2003_07