Reaktion #65917

ord-cbaaad8d1e694595b94773f37e5b580e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    workup.DISTILLATIONthe reaction mixture was distilled under reduced pressure
  3. 3
    Extraktionextracted with chloroform (80 ml×2 times)
  4. 4
    TrocknenThe organic layer was dried over anhydrous magnesiumsulfate
  5. 5
    workup.DISTILLATIONThe solvent was then distilled off under reduced pressure

Vorschrift

2-Formylfluorene (2.27 g, 11.7 mmol) and cycloheptylamine (1.39 g, 12.3 mmol) were heated together at 120° C. for 14 hrs. After cooling, the reaction mixture was distilled under reduced pressure. Then, ethanol (30 ml) and sodium borohydride (0.44 g, 11.7 mmol) were added to the residue and the mixture was stirred for 0.5 hr. The mixture was then diluted with water (100 ml) and extracted with chloroform (80 ml×2 times). The organic layer was dried over anhydrous magnesiumsulfate. The solvent was then distilled off under reduced pressure to give 3.15 g of a pale yellow solid residue.

Quelle

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