反应详情

To a solution of 6-bromo-N-[(1S)-1-(3-nitrophenyl)ethyl]pyridin-2-amine (100 mg, 0.31 mmol) in ethanol (5 mL) was added a solution of ammonium chloride (166 mg, 3.1 mmol) in water (2.5 mL), then indium powder (142 mg, mesh 100, 1.24 mmol). The mixture was heated at reflux for 4.5 hours, was allowed to cool to room temperature and was filtered through Celite. The filter cake was washed with water and ethanol and the combined filtrates were extracted with dichloromethane (2×30 mL) and the extracts washed with brine (30 mL), dried (Na2SO4) and concentrated under reduced pressure to give N-[(1S)-1-(3-aminophenyl)ethyl]-6-bromopyridin-2-amine (70 mg, 77%) as a dark yellow oil.

1. temperatureThe mixture was heated
2. temperatureat reflux for 4.5 hours
3. filtrationwas filtered through Celite
4. washThe filter cake was washed with water and ethanol
5. extractionthe combined filtrates were extracted with dichloromethane (2×30 mL)
6. washthe extracts washed with brine (30 mL)
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated under reduced pressure