Reaktion #46975

ord-3196d557fb8848f3bf1af18536d3e07f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto reflux for 15 h
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstigethe reaction mixture was evaporated
  4. 4
    Extraktionextracted by CH2Cl2
  5. 5
    TrocknenThe combined organic layer was dried by MgSO4
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigeto give a residue that
  8. 8
    Sonstigewas purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2)

Vorschrift

To a stirred solution of 18 (2 g, 4.84 mmol), AIBN (0.08 g, 0.48 mmol), Bu3SnH (3.91 ml, 14.50 mmol) in toluene (49 ml) was heated to reflux for 15 h. After cooling, the reaction mixture was evaporated and then extracted by CH2Cl2. The combined organic layer was dried by MgSO4 and concentrated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2) to give compound 19, yield 90%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741495B2uspto-grants-2010_06