反应详情

To a solution of 10.0 g (41.5 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 27.7 ml (200 mmol) of triethylamine in methylene chloride (100 ml), 8.86 g (49.8 mmol) of nicotinoyl chloride hydrochloride 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: methanol/ethyl acetate=1:10) to obtain powder. The powder was washed with ether and dried to obtain the desired compound (8.50 g, yield: 75.8%, pale 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: methanol/ethyl acetate=1:10)
7. customto obtain powder
8. washThe powder was washed with ether
9. customdried