HRID863972
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1.0 g (3.87 mmol) of 4-[3-(N-benzylamino)propylthio)-pyridine and 0.65 ml (4.64 mmol) of triethylamine in 25 ml of methylene chloride, 0.49 ml (4.64 mmol) of acetyl 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: chloroform/methanol=25:1) to obtain 980 mg of the desired compound (yield: 84.2%, yellow oil).
WORKUP
后处理
- temperaturecooling
- stirringThe mixture was stirred at room temperature for 30 minutes
- washThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water
- customdried
- distillationthe solvent was distilled off
- customThe residue was purified by column chromatography (eluent: chloroform/methanol=25:1)