反应详情

To a solution of 1.153 g (4.0 mmol) of 4-[2-(2-hydroxymethylbenzoyl)aminoethylthio]pyridine and 1.68 ml (12.1 mmol) of triethylamine in 50 ml of methylene chloride, 0.62 ml (8.0 mmol) of methanesulfonyl chloride was added with stirring at room temperature, and the mixture was stirred at room temperature for 30 minutes. The mixture was washed with saturated aqueous sodium bicarbonate, water 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 623 mg of the desired compound (57.6% yield, colorless crystals), mp. 86°-87° C.

1. stirringthe mixture was stirred at room temperature for 30 minutes
2. washThe mixture was washed with saturated aqueous sodium bicarbonate, water and saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled off
5. customthe residue was purified by column chromatography (eluent: ethyl acetate)