HRID863975

反应详情

EQUATION

反应方程式

HRID 863975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.62 g (6.24 mmol) of 4-[3-(N-2-pyridylmethylamino)propylthio]pyridine and 1.10 ml (7.80 mmol) of triethylamine in 10 ml of methylene chloride, 0.51 ml (7.80 mmol) of acetyl chloride was added under ice-cooling with stinting. 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 the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate/methanol=10:1) to obtain 1.61 g of the desired compound (yield: 85.6%, yellow oil).

WORKUP

后处理

  1. temperaturecooling with stinting
  2. washThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water
  3. customdried
  4. distillationthe solvent was distilled off
  5. customThe residue was purified by column chromatography (eluent: ethyl acetate/methanol=10:1)