Reaktion #90333

ord-e76fb66b66ca431fadcd51189f25119b

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe suspension was cooled to room temperature
  2. 2
    workup.STIRRINGto stir for overnight at room temperature
  3. 3
    FiltrationThe reaction was filtered through a fritted funnel
  4. 4
    EinengenThe filtrate was concentrated onto Celite®
  5. 5
    Sonstigepurified by reverse phase chromatography

Vorschrift

To a 20 mL vial, 2-(4-(1-(4-(perfluoroethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)acetyl azide (0.100 g, 0.228 mmol) was suspended in acetonitrile (1.5 mL). The suspension was stirred in a pre-heated heating block at 70° C. for 2 hours. The suspension was cooled to room temperature, then 2-isopropylaniline (0.0339 g, 0.251 mmol) and cesium carbonate (0.0890 g, 0.274 mmol) were added. The reaction was allowed to stir for overnight at room temperature. The reaction was filtered through a fritted funnel. The filtrate was concentrated onto Celite® and purified by reverse phase chromatography using 5-100% acetonitrile/water as eluent to provide the title compound as a white solid (0.028 g, 22%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09445594B2uspto-grants-2016_09