反应详情

In a two neck round bottom flask, 1-(naphthalene-2-ylsulfonyl)piperazine hydrochloride (compound 4, 0.72 mmoles, 0.200 g) and pyridine (7.22 mmoles, 2 mL) were charged in DCM (20 mL) at 0° C. CBZCl (1.08 mmoles, 0.30 g) was added slowly at the same temperature and then allowed the reaction mixture to stir for 3 h at room temperature. After completion of the reaction, water (10 mL) was added and extracted with DCM (2×20 mL). The combined organic layers were washed with brine (1×20 mL), dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by Column Chromatography (Silica gel 60-120, MeOH/DCM) to obtain the title compound (0.150 g, 50.6%) as an off-white solid.

1. additionwas added
2. extractionextracted with DCM (2×20 mL)
3. washThe combined organic layers were washed with brine (1×20 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by Column Chromatography (Silica gel 60-120, MeOH/DCM)