反应详情

To a stirred mixture of (trans)-3-azido-4-fluoropyrrolidine (18 g) in CH2Cl2 (120 mL) was added DIPEA (35 g, 0.27 mol, 2.5 eq), then CBZ-Cl (22 g, 0.13 mol) was added dropwise at 0-5° C. After addition, the resulting mixture was stirred at rt overnight. The mixture was washed with sat. aq. NH4Cl (150 mL), sat. aq. NaHCO3 (3×40 mL) and brine (40 mL). The organic layer was concentrated and purified by column (petroleum ether/EtOAc=10:1˜5:1) to give the title compound (30 g, ˜100% yield in two steps, containing residual EtOAc and DCM) as a light yellow oil.

1. additionAfter addition
2. washThe mixture was washed with sat. aq. NH4Cl (150 mL), sat. aq. NaHCO3 (3×40 mL) and brine (40 mL)
3. concentrationThe organic layer was concentrated
4. custompurified by column (petroleum ether/EtOAc=10:1˜5:1)