反应详情

To a solution of 700 mg (4.60 mmol) of 4-(3-aminopropyloxy)pyridine and 1.54 ml (11.0 mmol) of triethylamine in 30 ml of methylene chloride, 830 mg (4.66 mmol) of nicotinoyl chloride hydrochloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:10 to 1:5) to obtain 1.05 g of the desired compound (yield: 85.8%, colorless crystals). mp: 117°-119° C.

1. temperaturecooling
2. stirringThe mixture was stirred at room temperature for 1.5 hours
3. washThe reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off
6. customThe residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:10 to 1:5)