反应详情

温度

80 °C

[1-(4-Nitro-benzenesulfonyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (0.5 g, 1.3 mmol) was suspended in a 5:1 mixture of ethanol and water (20 ml). To this solution was added iron powder (0.22 g, 3.4 mmol) followed by saturated ammonium chloride solution (3 ml) and the mixture was heated to 80° C. for three hours. After this time, the reaction mixture was cooled to room temperature and filtered through a pad of celite, the celite was washed with ethanol (10 ml) and EtOAc (50 ml) and the solution was concentrated under vacuum. The resulting residue was suspended in water (10 ml) and the solid precipitate collected by filtration and dried under vacuum to give the title compound (0.38 g, 78% yield) as a white solid. Tr=1.84 min, m/z (ES+) (M+Na)+ 378.

1. temperatureAfter this time, the reaction mixture was cooled to room temperature
2. filtrationfiltered through a pad of celite
3. washthe celite was washed with ethanol (10 ml) and EtOAc (50 ml)
4. concentrationthe solution was concentrated under vacuum
5. filtrationthe solid precipitate collected by filtration
6. customdried under vacuum