反应详情

温度

45 °C

0.70 g (10.76 mmol) of sodium azide was added to 1.56 g (8.42 mmol) of 1-(methylsulfinyl)-4-nitrobenzene in 20 ml DCM. 2.3 ml concentrated sulfuric acid was slowly added to the mixture at 0° C. and it was then heated to 45° C. After 16 h the mixture was cooled to room temperature, and after adding water it was extracted with DCM. The aqueous phase was adjusted to pH 11 with 15% sodium hydroxide solution and extracted with DCM (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. 1.08 g (5.39 mmol; yield: 63%) of the product was obtained.

1. temperatureAfter 16 h the mixture was cooled to room temperature
2. extractionwas extracted with DCM
3. extractionextracted with DCM (2×)
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated by evaporation
7. custom1.08 g (5.39 mmol; yield: 63%) of the product was obtained