反应详情

温度

80 °C

To a solution of 5,6-difluoro-1H-indole-3-carbaldehyde (1.0 g) in tetrahydrofuran (15 ml) were added hydroxylamine hydrochloride (0.81 g) and pyridine (1.9 g), and this mixture was stirred at 80° C. for 8 hours. Acetic anhydride was added to reaction mixture and this mixture was stirred at 80° C. for 8 hours. After cooling to ambient temperature, 2 mol/L aqueous sodium hydroxide solution was added to this mixture and resulting mixture was stirred for 30 minutes. This mixture was poured into 2 mol/L hydrochloric acid and the precipitated solid was collected by filtration, and washed with water and n-hexane. The solid was dissolved in ethyl acetate and this residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (0.95 g).

1. stirringthis mixture was stirred at 80° C. for 8 hours
2. temperatureAfter cooling to ambient temperature
3. customresulting mixture
4. stirringwas stirred for 30 minutes
5. filtrationthe precipitated solid was collected by filtration
6. washwashed with water and n-hexane
7. dissolutionThe solid was dissolved in ethyl acetate
8. customthis residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate)