HRID428132

反应详情

EQUATION

反应方程式

HRID 428132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of trans-3-(3-pyridyl)acrylic acid (179 g) in dichloromethane (4.8 L), triethylamine (584 ml) and pivaloyl chloride (148 ml) were sequentially added under ice-cooling and stirring and stirred for 15 minutes. Subsequently, 3-hydroxyphenethylamine hydrobromide (263 g) was added at the same temperature and stirred for 2 hours. After the solvent was distilled out under reduced pressure, water was added to the residue and the precipitated crystal was filtered, washed with water and recrystallized in ethanol to yield the titled compound (251.4 g, 78%).

WORKUP

后处理

  1. temperaturecooling
  2. stirringstirred for 15 minutes
  3. stirringstirred for 2 hours
  4. distillationAfter the solvent was distilled out under reduced pressure, water
  5. additionwas added to the residue
  6. filtrationthe precipitated crystal was filtered
  7. washwashed with water
  8. customrecrystallized in ethanol