Reaktion #84133
ord-13bddc8cdb4744b6adca3a3f2e2664b0
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas added
- 2Temperaturthe mixture heated
- 3Temperaturto reflux for 15 h
- 4SonstigeThe reaction was quenched with saturated aqueous sodium sulfate at 0° C.
- 5Filtrationthe reaction mixture filtered
- 6TrocknenThe filtrate was dried over anhydrous sodium sulfate
- 7Sonstigeevaporated to dryness
- 8Sonstigeto afford solid, which
- 9Waschenwas washed with water
- 10Sonstigedried
Vorschrift
Lithium aluminum hydride (3 g, 78.95 mmol) was placed in 1,4-dioxane (100 mL) under inert atmosphere and 9-methyl-2,3,4,5-tetrahydroazepino[4,3-b]indol-1(6H)-one (3 g, 14.018 mmol) was added, and the mixture heated to reflux for 15 h. The reaction was monitored by TLC. The reaction was quenched with saturated aqueous sodium sulfate at 0° C., and the reaction mixture filtered. The filtrate was dried over anhydrous sodium sulfate and evaporated to dryness to afford solid, which was washed with water followed by EtOAc, and dried to afford 1.25 g of the title compound.