反应详情

To a solution of 4.03 g (15.0 mmol) of 4-[3-(t-butoxycarbonylamino)propylthio]pyridine in 100 ml of methylene chloride, 3.05 g (15.0 mmol) of m-chloroperbenzoic acid was added with stirring under ice-cooling, and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was washed two times with saturated aqueous sodium bicarbonate and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10 : 1) to give 3.37 g of the desired compound (78.9% yield, colorless crystals).

1. temperaturecooling
2. stirringthe mixture was stirred at the same temperature for 1 hour
3. washThe reaction mixture was washed two times with saturated aqueous sodium bicarbonate
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off
6. customthe residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10 : 1)