反应详情

温度

80 °C

12.0 g 6-nitro-2-phenyl-3H-imidazo[4,5-b]pyridine were dissolved in 1 l acetic acid. 18 g iron powder were added and the mixture heated to 80° C. with stirring. After 2 hrs the mixture was cooled to room temperature and filtered over Celite. The celite pad was washed with methanol and the combined filtrates were evaporated. The residue was dissolved methanol/dichloromethane 1:1 and filtered over silica. The filtrate was concentrated to a volume of 100 ml, the resulting precipitate collected by filtration and washed with methanol.

1. temperatureAfter 2 hrs the mixture was cooled to room temperature
2. filtrationfiltered over Celite
3. washThe celite pad was washed with methanol
4. customthe combined filtrates were evaporated
5. dissolutionThe residue was dissolved methanol/dichloromethane 1:1
6. filtrationfiltered over silica
7. concentrationThe filtrate was concentrated to a volume of 100 ml
8. filtrationthe resulting precipitate collected by filtration
9. washwashed with methanol