Reaktion #67150

ord-d2a66c4f8b3a4b0bab6ec1cc561e84d1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated under a stream of nitrogen
  2. 2
    Sonstigethe residue partitioned between ethyl acetate (10 ml) and saturated ammonium chloride (5 ml)
  3. 3
    SonstigeThe organic layer was separated by hydrophobic frit
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigethe solvent removed in vacuo
  6. 6
    SonstigeThe residual solid was purified by Mass Directed Automated Preparative HPLC (Method B)
  7. 7
    Sonstigethe solvent was evaporated under a stream of nitrogen

Vorschrift

Sodium hydroxide (2 ml, 4.00 mmol) was added to a solution of N-[5-[4-(5-{[(2R,6S)-2,6-dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide (194 mg, 0.212 mmol) in 1,4-dioxane (2 ml). The mixture was stirred at room temperature for 2 h. The solvent was evaporated under a stream of nitrogen and the residue partitioned between ethyl acetate (10 ml) and saturated ammonium chloride (5 ml). The organic layer was separated by hydrophobic frit, washed with water and the solvent removed in vacuo. The residual solid was purified by Mass Directed Automated Preparative HPLC (Method B) and the solvent was evaporated under a stream of nitrogen to give the title compound as a cream coloured solid (10 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524751B2uspto-grants-2013_09