反应详情

温度

75 °C

To a solution of tert-butyl 4-(4-((tert-butoxycarbonyl (2-chloro-5-methoxy-4-nitrophenethyl)amino)methyl)phenyl)piperazine-1-carboxylate (0.480 g, 0.793 mmol) in methanol (15 mL), a saturated solution of NH4Cl (10 mL) and zinc powder (0.257 g, 3.96 mmol) were added at room temperature and the reaction stirred at 70-80° C. for 1 hour. The mixture was allowed to cool to room temperature and filtered through a celite pad. Water (40 mL) was added to the filtrate and the mixture extracted with EtOAc (2×30 mL). The combined organic extracts were washed with brine (10 mL), dried (Na2SO4) and concentrated under reduced pressure to give the title compound (0.440 g, 97%).

1. temperatureto cool to room temperature
2. filtrationfiltered through a celite pad
3. additionWater (40 mL) was added to the filtrate
4. extractionthe mixture extracted with EtOAc (2×30 mL)
5. washThe combined organic extracts were washed with brine (10 mL)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated under reduced pressure