反应详情

温度

0 °C

A solution of NaNO2 (0.015 g, 0.216 mmol) in water (1.5 mL) was added to an ice-cold solution of Example 26 (0.075 g, 0.212 mmol) in HCl (3 mL, 37% w/v) over 10 minutes. A solution of NaN3 (0.138 g, 2.12 mmol) in water (0.5 mL) was added drop wise with stirring at 0° C. over 10 minutes, and the temperature of the mixture was allowed to rise to 25° C. After stirring for another 20 minutes at room temperature, the mixture was extracted with DCM (3×25 mL), and the combined organic extracts were dried (Na2SO4), filtered and concentrated under reduced pressure to provide the titled compound. MS (ESI) m/z 381 (M+H); IR: 2097 cm−1.

1. customto rise to 25° C
2. stirringAfter stirring for another 20 minutes at room temperature
3. extractionthe mixture was extracted with DCM (3×25 mL)
4. dry with materialthe combined organic extracts were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure