Reaktion #42094

ord-0bd540e1a1ed4deb903c402c40db425f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereaction
  2. 2
    workup.WAITThe temperature was elevated to 50° C. for 6 hours at which
  3. 3
    Waschenwashed with saturated aqueous NaHCO3 solution
  4. 4
    EinengenThe solution was concentrated
  5. 5
    Sonstigepurified via flash chromatography on silica gel with a gradient elution of 0% to 15% EtOAc in hexane affording the title compound

Vorschrift

To the product of Step C EXAMPLE 26 (300 mg) in THF (3.3 mL) was added isobutylamine (0.83 mL). The reaction stirred at room temperature overnight at which point LC/MS indicated incomplete reaction. The temperature was elevated to 50° C. for 6 hours at which point the reaction was diluted with EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 15% EtOAc in hexane affording the title compound. HPLC/MS: 396.1 (M+1), 398.1 (M+3); Rt=4.77 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728141B2uspto-grants-2010_06