反应详情

温度

100 °C

A mixture of 1-benzhydryl-3-chloro-3-methyl-azetidine (2 g, 7.39 mmol) and NaN3 (0.8 g, 12.31 mmol) was dissolved in DMF (30 mL) and the mixture was stirred at 100° C. overnight. The mixture was cooled to ambient temperature and partitioned between water (150 mL) and DCM (50 mL). The organic phase was washed with brine (3×30 mL), dried over anhydrous Na2SO4 and concentrated in vacuo to give 3-azido-1-benzhydryl-3-methyl-azetidine as a yellow oil (2.1 g, 100%), which was used directly in the next step. LC/MS (Table 1, Method 2) Rt=0.915 min; MS m/z: 279 [M+H]+

1. temperatureThe mixture was cooled to ambient temperature
2. custompartitioned between water (150 mL) and DCM (50 mL)
3. washThe organic phase was washed with brine (3×30 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo