HRID535667
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
A solution of 2-(6-methoxypyridin-2-yl)ethanol (0.23 g, 1.50 mmol), 4-dimethylaminopyridine (0.028 g, 0.23 mmol), triethylamine (0.63 mL, 4.50 mmol) and p-toluenesulfonyl chloride (0.34 g, 1.80 mmol) in dry dichloromethane (5 mL) was stirred at rt over night. The solvent was removed in vacuo. Ethyl acetate and water were added. The organic phase was separated and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried (Na2SO4) and concentrated. The product was purified by flash chromatography (SiO2; heptane/EtOAc, gradient 0-100%). Yield: 0.18 g (38%).
WORKUP
后处理
- customThe solvent was removed in vacuo
- additionEthyl acetate and water were added
- customThe organic phase was separated
- extractionthe aqueous phase was extracted with ethyl acetate
- dry with materialThe combined organic phases were dried (Na2SO4)
- concentrationconcentrated
- customThe product was purified by flash chromatography (SiO2; heptane/EtOAc, gradient 0-100%)