Reaktion #1359293
ord-650fddfa47e74d4fb356d9324a5eea60
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturunder reflux for 15 min
- 2Extraktionextracted with ethyl acetate
- 3FiltrationAfter filtration over speedex the phases
- 4Sonstigewere separated
- 5Extraktionthe aqueous phase was extracted twice with ethyl acetate
- 6WaschenThe combined organic layers were washed with brine
- 7Trocknendried over magnesium sulfate
- 8Sonstigeevaporated
- 9SonstigeThe so-obtained product was used without further purification
Vorschrift
To a stirred suspension of 5 mL tert-butyl methyl ether and 0.14 g (3.68 mmol) lithium aluminium hydride was added 0.23 g (0.92 mmol) (R)-6-chloro-4,7-dimethyl-3,4-dihydro-2H-2,4a,5-triaza-fluoren-1-one. The suspension was stirred under reflux for 15 min and, after cooling to room temperature, was poured into saturated aqueous sodium potassium tartrate solution and extracted with ethyl acetate. After filtration over speedex the phases were separated and the aqueous phase was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate and evaporated. The so-obtained product was used without further purification.