Reaktion #46364

ord-a91e682d1e5f4f50b13ded6fe34a9d27

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe reaction solution was partitioned between ethyl acetate and water
  3. 3
    WaschenThe organic layer was washed with water, saturated brine
  4. 4
    Sonstigedried
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeThe residue was chromatographed over silica gel
  7. 7
    Wascheneluting with a gradient of 10 to 50% ethyl acetate in hexane

Vorschrift

(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (0.607 g), and 2-chloro-6,7-difluoroquinoxaline McQuaid et. al. J. Med. Chem. (1992), 35(18), 3319-24 (0.569 g) were dissolved in dimethylformamide (1 ml) and heated to 90° C. for 5 days under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with water, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 10 to 50% ethyl acetate in hexane. The title compound was obtained as a pale yellow solid (0.460 g), MH+ 379.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741329B2uspto-grants-2010_06