HRID1627780
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
In a flask equipped by a Dean-Stark trap, a mixture of ethyl levulinate (28.83 g; 200 mmol), ethylene glycol (37.24 g; 600 mmol) and a catalytic amount of pyridinium para-toluenesulfonic acid in toluene (200 mL) was heated at reflux until the theoretical amount of water was distilled off. After cooling, the mixture was washed with a saturated solution of sodium hydrogenocarbonate. The basic layer was extracted with diethylether and the organics were combined, then washed with brine and water. The organic layer was dried over sodium sulphatesulphate and concentrated under reduced pressure to afford the ethyl 3-(2-methyl-1,3-dioxolan-2-yl)propanoate as a colorless oil.
WORKUP
后处理
- customIn a flask equipped by a Dean-Stark trap
- distillationwas distilled off
- temperatureAfter cooling
- washthe mixture was washed with a saturated solution of sodium hydrogenocarbonate
- extractionThe basic layer was extracted with diethylether
- washwashed with brine and water
- dry with materialThe organic layer was dried over sodium sulphatesulphate
- concentrationconcentrated under reduced pressure