反应详情

Sodium hydride (60% in oil, 228 mg, 5.7 mmol) was gradually added to a N,N-dimethylformamide (0.5 ml) solution of 5-nitroindole (0.841 g, 5.19 mmol) while stirring at room temperature; phenyl N-methylcarbamate (1.02 g, 6.74 mmol) was added thereto; and the reaction mixture was stirred overnight. The reaction mixture was partitioned between ethyl acetate and water; and the organic layer was washed with water and brine, dried over anhydrous sodium sulfate. This was concentrated under reduced pressure; and the residue was purified by silica gel column chromatography (hexane-ethyl acetate, sequentially ethyl acetate) to yield the title compound (600 mg).

1. stirringand the reaction mixture was stirred overnight
2. customThe reaction mixture was partitioned between ethyl acetate and water
3. washand the organic layer was washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationThis was concentrated under reduced pressure
6. customand the residue was purified by silica gel column chromatography (hexane-ethyl acetate, sequentially ethyl acetate)