Reaktion #86082

ord-c9593268eace46aabd296c24083a8a59

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturthe mixture heated
  3. 3
    Temperaturto reflux for 15 h
  4. 4
    SonstigeThe reaction was quenched with saturated aqueous sodium sulfate at 0° C.
  5. 5
    Filtrationthe reaction mixture filtered
  6. 6
    TrocknenThe filtrate was dried over anhydrous sodium sulfate
  7. 7
    Sonstigeevaporated to dryness
  8. 8
    Sonstigeto afford solid, which
  9. 9
    Waschenwas washed with water
  10. 10
    Sonstigedried

Vorschrift

Lithiumaluminum hydride (3 g, 78.95 mmol) was placed in 1,4-dioxane (100 mL) under inert atmosphere and 9-methyl-2,3,4,5-tetrahydroazepino[4,3-b]indol-1(6H)-one (3 g, 14.018 mmol) was added, and the mixture heated to reflux for 15 h. The reaction was monitored by TLC. The reaction was quenched with saturated aqueous sodium sulfate at 0° C., and the reaction mixture filtered. The filtrate was dried over anhydrous sodium sulfate and evaporated to dryness to afford solid, which was washed with water followed by EtOAc, and dried to afford 1.25 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434747B2uspto-grants-2016_09