HRID246044
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of (2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (1.25 g, 9.46 mmol) and triethylamine (9.2 ml, 66.2 mmol) in dichloromethane (60 ml) at 0° C. was slowly added methanesulfonyl chloride (2.2 ml, 28.4 mmol). The reaction mixture was stirred at 0° C. for 2 h then quenched with water and the aqueous layer was extracted with dichloromethane. The combined organics were washed with 10% citric acid, sat NaHCO3, and brine then dried over MgSO4 and concentrated to afford methanesulfonic acid 2,2-dimethyl-[1,3]dioxolan-4-ylmethyl ester as a light brown oil which was used without further purification.
WORKUP
后处理
- customat 0° C.
- customthen quenched with water
- extractionthe aqueous layer was extracted with dichloromethane
- washThe combined organics were washed with 10% citric acid
- dry with materialthen dried over MgSO4
- concentrationconcentrated