反应详情

To a solution of 2.00 g (8.29 mmol) of 3-(3-aminopropylthio)pyridine dihydrochloride and 4.16 ml (29.9 mmol) of triethylamine in 80 ml of methylene chloride, 1.06 ml (9.95 mmol) of 2-thenoyl chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain powder. The powder was washed with ether and dried to obtain 1.97 g of the desired compound (yield: 85.3%, yellow powder).

1. temperaturecooling
2. stirringThe mixture was stirred at room temperature for 30 minutes
3. washThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water
4. customdried
5. distillationthe solvent was distilled off
6. customThe residue was purified by column chromatography (eluent: ethyl acetate)
7. customto obtain powder
8. washThe powder was washed with ether
9. customdried