HRID1830124
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
- 49 °C
PROCEDURE
实验过程
A solution of 2,2-bis-(2-phenylsulfanyl-ethyl)-malonic acid diethyl ester (5.614 g) in ethanol (100 mL) was treated with lithium hydroxide (2.84 g) in water (10 mL). The reaction mixture was heated at 49° C. for 17 hours followed by 85° C. for 2 hours. The solvents were evaporated at reduced pressure to give a residue that was treated with water (100 mL) and washed with ether. The aqueous layer was cooled on ice, acidified and the product extracted with ethyl acetate. The extracts were dried over magnesium sulfate. The solvent was removed by rotary evaporation at reduced pressure to give acid 2,2-bis-(2-phenylsulfanyl-ethyl)-malonic acid (5.628 g).
WORKUP
后处理
- customThe solvents were evaporated at reduced pressure
- customto give a residue that
- washwashed with ether
- temperatureThe aqueous layer was cooled on ice
- extractionthe product extracted with ethyl acetate
- dry with materialThe extracts were dried over magnesium sulfate
- customThe solvent was removed by rotary evaporation at reduced pressure