Reaktion #338568

ord-7284b8516f8b4b01a7035d4680ac6e20

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Waschenthe resulting solution was washed twice with brine
  3. 3
    SonstigeAfter evaporation of the organic phase
  4. 4
    Sonstigethe resulting residue was purified by flash chromatography (Acros Silicagel 0.060-0.200 mm)

Vorschrift

18 g compound 19 (86 mmole), 20.8 g ureum (346 mmole) and 5 drops polyphosphoric acid were heated at 150° C. during 18 h. After cooling, 500 ml EtOAc was added and the resulting solution was washed twice with brine. After evaporation of the organic phase, the resulting residue was purified by flash chromatography (Acros Silicagel 0.060-0.200 mm) using cyclohexane/isopropanol 95:5, affording compound 20 as a white powder (9.17 g, 51% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07863428B2uspto-grants-2011_01