反应详情

To a solution of 1.00 g (5.49 mmol) of 4-(4-aminobutylthio)pyridine and 0.92 ml (6.60 mmol) of triethylamine in 30 ml of methylene chloride, 0.67 ml (5.77 mmol) of benzoyl chloride was added with stirring under ice-cooling and the mixture was stirred at room temperature for 13 hours. The mixture was washed with saturated aqueous sodium bicarbonate and saturated saline, and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate) to give 0.54 g of the desired compound (34.4% yield, colorless crystals), mp. 75°-77° C.

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 13 hours
3. washThe mixture was washed with saturated aqueous sodium bicarbonate and saturated saline
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)