Reaktion #65917
ord-cbaaad8d1e694595b94773f37e5b580e
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2workup.DISTILLATIONthe reaction mixture was distilled under reduced pressure
- 3Extraktionextracted with chloroform (80 ml×2 times)
- 4TrocknenThe organic layer was dried over anhydrous magnesiumsulfate
- 5workup.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.