HRID428132
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 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
- temperaturecooling
- stirringstirred for 15 minutes
- stirringstirred for 2 hours
- distillationAfter the solvent was distilled out under reduced pressure, water
- additionwas added to the residue
- filtrationthe precipitated crystal was filtered
- washwashed with water
- customrecrystallized in ethanol