反应详情

温度

45 °C

23.65 g (127.7 mmol) (RS)-1-(methylsulfinyl)-4-nitrobenzene in 130 ml chloroform are treated with 9.32 g (143.4 mmol) sodium azide. The mixture is slowly treated with 32.4 ml of concentrated sulfuric acid at 0° C. and then slowly heated to 45° C. After 16 hrs, the mixture is cooled to room temperature, treated with ice-water and extracted with chloroform. This organic phase is discarded. The aqueous phase is basified with 2N NaOH solution and extracted with DCM. The combined organic phases are washed with saturated NaCl solution, dried (Na2SO4), filtered and concentrated. 17.17 g (88.4 mmol, corresponding to 63% of theor.) of the product is obtained.

1. temperaturethe mixture is cooled to room temperature
2. extractionextracted with chloroform
3. extractionextracted with DCM
4. washThe combined organic phases are washed with saturated NaCl solution
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. custom17.17 g (88.4 mmol, corresponding to 63% of theor.) of the product is obtained