反应详情

The product from Example H (3.90 g, 8.42 mmol) was suspended in 50 mL of 20% piperidine in dichloromethane at room temperature with stirring (2 h). The solution was concentrated under reduced pressure and partitioned between ethyl acetate and water (100 mL each) and separated. The organic layer was washed with 5% sodium bicarbonate (2×50 mL), brine (2×50 mL), dried with magnesium sulfate, filtered and concentrated under reduced pressure to an oil. The oil was purified by silica gel chromatography with ethyl acetate and methanol (3:1). Appropriate fractions were combined and concentrated under reduced pressure to a solid (1.34 g).

1. concentrationThe solution was concentrated under reduced pressure
2. custompartitioned between ethyl acetate and water (100 mL each)
3. customseparated
4. washThe organic layer was washed with 5% sodium bicarbonate (2×50 mL), brine (2×50 mL)
5. dry with materialdried with magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure to an oil
8. customThe oil was purified by silica gel chromatography with ethyl acetate and methanol (3:1)
9. concentrationconcentrated under reduced pressure to a solid (1.34 g)