反应详情

温度

65 °C

A flask equipped with an overhead stirrer, thermometer and reflux condenser was placed under a nitrogen atmosphere then charged with the epoxide of Example 5 (20.0 g, 118 mmol), sodium azide (NaN3; 31.0 g, 473 mmol), magnesium sulfate (MgSO4; 14.0 g, 118 mmol) and methanol (MeOH; 200 mL). The mixture was heated to 65±5° C. for 2 hours then cooled to 25±5° C. and filtered through a pad of Celite 545. The solvent was removed under reduced pressure resulting in a thick oil which was taken up in IPAc (250 mL) then washed with water (3×250 mL). The organic phase was dried over sodium sulfate (Na2SO4), filtered and concentrated under reduced pressure to provide the title compound (15.1 g, 60%) as a white solid.

1. customA flask equipped with an overhead stirrer
2. temperaturethermometer and reflux condenser
3. temperaturethen cooled to 25±5° C.
4. filtrationfiltered through a pad of Celite 545
5. customThe solvent was removed under reduced pressure
6. customresulting in a thick oil which
7. washthen washed with water (3×250 mL)
8. dry with materialThe organic phase was dried over sodium sulfate (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure