Reaktion #1359293

ord-650fddfa47e74d4fb356d9324a5eea60

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 15 min
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    FiltrationAfter filtration over speedex the phases
  4. 4
    Sonstigewere separated
  5. 5
    Extraktionthe aqueous phase was extracted twice with ethyl acetate
  6. 6
    WaschenThe combined organic layers were washed with brine
  7. 7
    Trocknendried over magnesium sulfate
  8. 8
    Sonstigeevaporated
  9. 9
    SonstigeThe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07208494B2uspto-grants-2007_04