反应详情

温度

60 °C

A solution of 5-methoxy-3,3-dimethyl-indane-1-one (Intermediate 16, 3.3 g, 17.4 mmol) in benzene (50 mL) was treated with concentrated sulfuric acid (10 mL) and heated to 60° C. Sodium azide (1.95 g, 30 mmol) was added in small portions and after the addition was complete, the reaction mixture was heated further for 4 h. It was then cooled, diluted with water and extracted with chloroform (×3). The combined organic phase was dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to afford the title compound as a brown solid (3.5 g, quantitative by weight).

1. additionafter the addition
2. temperaturethe reaction mixture was heated further for 4 h
3. temperatureIt was then cooled
4. extractionextracted with chloroform (×3)
5. dry with materialThe combined organic phase was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customevaporated in vacuo