反应详情

To a suspension of sodium hydride (60%, 0.05 g (1.25 mmol)) in DMF (2.0 ml), 4′-fluoro-2′-nitro-p-toluenesulfonanilide (0.31 g (1.00 mmol)) was added with stirring at room temperature. To the resulting mixture, after 15 minutes' stirring at room temperature, ethyl iodide (0.30 ml (3.75 mmol)) was added dropwise. After 30 minutes' heating at 100° C. with stirring, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water and saturated sodium chloride solution, successively, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. Diisopropyl ether was added to the residue and the solid separated was filtered and washed to give 0.25 g (74%) of the title compound as pale yellow crystals.

1. additionwas added
2. stirringTo the resulting mixture, after 15 minutes' stirring at room temperature
3. temperatureAfter 30 minutes' heating at 100° C.
4. stirringwith stirring
5. extractionextracted with ethyl acetate
6. washThe extract was washed with water and saturated sodium chloride solution
7. dry with materialsuccessively, dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionDiisopropyl ether was added to the residue
10. customthe solid separated
11. filtrationwas filtered
12. washwashed