Reaktion #307091

ord-58d1b9bc56184252b8f9057383d3023d

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe title compound was prepared following procedure
  2. 2
    FiltrationThe reaction mixture was filtered through a SPE NH2 column (2 g)
  3. 3
    Waschenrinsed with ACN
  4. 4
    Waschenrinsed with ACN
  5. 5
    SonstigeAfter evaporation of the solvents
  6. 6
    Sonstigethe crude product was purified by flash chromatography (c-hex/EtOAc: 9.5/0.5)

Vorschrift

The title compound was prepared following procedure described for example 4, step 1, but starting from Intermediate 3 (113.1 mg; 0.50 mmol; 1 eq.) and Intermediate 2 (106.1 mg; 0.50 mmol; 1 eq.). The reaction mixture was filtered through a SPE NH2 column (2 g) and rinsed with ACN. The filtrate was passed through a SPE SCX column (2 g) and rinsed with ACN. After evaporation of the solvents, the crude product was purified by flash chromatography (c-hex/EtOAc: 9.5/0.5), affording the title compound as a off-white solid. LC/MS (Method A): 403.0 (M+H)+. HPLC (Method A) Rt 6.20 min (Purity: 96.8%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08202865B2uspto-grants-2012_06