Reaktion #65922

ord-bcd683ca1d504603831d112f5f722637

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONdistilled under reduced pressure
  2. 2
    Extraktionextracted with chloroform (80 ml×2 times)
  3. 3
    TrocknenThe organic layer was dried over anhydrous magnesium sulfate
  4. 4
    Einengenconcentrated
  5. 5
    SonstigeThe residue was then purified by silica gel column chromatography

Vorschrift

2-Acetylfluorene (4.17 g, 20 mmol) and cycloheptylamine (2.38 g, 21 mmol) were heated together at 130° C. for 14 hrs and, then, distilled under reduced pressure. To the residue were added ethanol (20 ml) and sodium borohydride (0.76 g, 20 mmol) and the mixture was stirred at room temperature overnight. The mixture was then diluted with water (100 ml) and extracted with chloroform (80 ml×2 times). The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was then purified by silica gel column chromatography to give 1.58 g of the amine compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420348uspto-grants-1995_05