反应详情

To a suspension of sodium hydride (60%, 0.24 g (6.00 mmol)) in DMF (8.0 ml), N-(2,4-dinitrophenyl)-O-methylhydroxylamine (0.85 g (3.99 mmol)) was added under ice-cooling with stirring. After 15 minutes' stirring under ice-cooling, p-toluenesulfonyl chloride (1.15 g (6.03 mmol)) was added. Then, the temperature of the reaction mixture was brought to room temperature and stirred at the same temperature for 18 hours. The reaction mixture was then 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. The residue was subjected to silica gel chromatography with ethyl acetate-hexane (1:3) as eluent, to give 0.30 g (21%) of the title compound as orange crystals.

1. additionwas added under ice-
2. temperaturecooling
3. stirringAfter 15 minutes' stirring under ice-
4. temperaturecooling
5. customwas brought to room temperature
6. stirringstirred at the same temperature for 18 hours
7. extractionextracted with ethyl acetate
8. washThe extract was washed with water and saturated sodium chloride solution
9. dry with materialsuccessively, dried over anhydrous magnesium sulfate
10. concentrationconcentrated under reduced pressure