Reaktion #59245

ord-d9827e1b6c9b4e9983e0a8ae85e58b4c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is refluxed for 2 h
  2. 2
    Sonstigeevaporated
  3. 3
    Sonstigethe crude mixture purified by RP HPLC on a Phenominex column (250×20 mm)
  4. 4
    Sonstigeover 30 minutes

Vorschrift

The compound from Step 2 is suspended in dry ethanol and O-trimethylsilyl hydroxylamine (10 eq.) is added. The mixture is refluxed for 2 h, evaporated and the crude mixture purified by RP HPLC on a Phenominex column (250×20 mm) using a gradient of acetonitrile in water from 0 to 30% over 30 minutes at 10 mL/minute to yield the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425547B2uspto-grants-2008_09