反应详情

The title compound was prepared by following general procedure 1. p-Tolyl hydrazine hydrochloride (15 g, 94.55 mmol) was taken into 7% H2SO4 in 1,4-dioxane (650 mL), 1-methylazepan-4-one.HCl (15.4 g, 94.55 mmol) was added and stirred at RT for 10 min. The reaction mixture was stirred at 80° C. for 14 h. After completion of the reaction, reaction mass was slowly basified with 50% NaOH solution, extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated to dryness and purified by column chromatography (silica gel 100-200 mesh; eluent: 10% methanol-DCM) to afford 3,9-dimethyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole (5 g).

1. customThe title compound was prepared
2. stirringThe reaction mixture was stirred at 80° C. for 14 h
3. customAfter completion of the reaction, reaction mass
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. customevaporated to dryness
7. custompurified by column chromatography (silica gel 100-200 mesh; eluent: 10% methanol-DCM)