반응 #86082

반응 방정식

Lithiumaluminum hydride

9-methyl-2,3,4,5-tetrahydroazepino[4,3-b]indol-1(6H)-one

1,4-dioxane

→

title compound

2,9-dimethyl-1,2,3,4,5,6-hexahydroazepino[4,3-b]indole

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도the mixture heated
3. 3
   온도to reflux for 15 h
4. 4
   기타The reaction was quenched with saturated aqueous sodium sulfate at 0° C.
5. 5
   여과the reaction mixture filtered
6. 6
   건조The filtrate was dried over anhydrous sodium sulfate
7. 7
   기타evaporated to dryness
8. 8
   기타to afford solid, which
9. 9
   세척was washed with water
10. 10
    기타dried

실험 절차

Lithiumaluminum 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.

출처