反应详情

温度

0 °C

The product of Example 76A (4.00 g, 19.4 mmol) in acetone (9 mL) at 0° C. was treated with a solution of sodium azide (1.27 g) in water (9 mL) dropwise over 15 minutes. After stirring for 30 minutes at 0° C., the mixture was extracted with toluene (20 mL). The organic extract was dried with MgSO4, filtered, and the filtrate heated at reflux for 1 hour. The mixture was allowed to cool to room temperature and was concentrated under reduced pressure to provide the title compound as a pale yellow oil (3.45 g, 96%).

1. extractionthe mixture was extracted with toluene (20 mL)
2. extractionThe organic extract
3. dry with materialwas dried with MgSO4
4. filtrationfiltered
5. temperaturethe filtrate heated
6. temperatureat reflux for 1 hour
7. temperatureto cool to room temperature
8. concentrationwas concentrated under reduced pressure