Reaktion #162760

ord-0a7a392b929240649a560159c1c399f7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was then filtered through Celite
  2. 2
    Waschenwashing with ethanol
  3. 3
    Sonstigeevaporated to dryness
  4. 4
    SonstigeThe residue was purified by FCC
  5. 5
    Wascheneluting with 0-10% MeOH in DCM

Vorschrift

Intermediate 6a (212 mg, 1.04 mmol) was dissolved in ethanol (20 mL) then hydrogenated over 10% palladium on carbon for 4 h under hydrogen atmosphere. The mixture was then filtered through Celite, washing with ethanol, and evaporated to dryness. The residue was purified by FCC, eluting with 0-10% MeOH in DCM, to give the title compound as a pale brown solid (154 mg, 86%). LCMS (Method 3): Rt 1.92 min, m/z 174.1 [MH−].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835431B2uspto-grants-2014_09