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
- 130 °C
PROCEDURE
实验过程
345 mg of 3-trifluoromethylnonyl p-toluenesulfonate obtained in Step (1), 166 mg of ethyl p-hydroxybenzoate and 1 ml of dimethylformamdie (DMF) were placed in a round-bottomed flask, and 80 mg of sodium hydride (60%) was added thereto together with DMF, followed by 6 hours of stirring at 130° C. After the reaction, DMF was distilled off under a reduced pressure, and water was added, followed by extraction with methylene chloride. The methylene chloride solution was dried with magnesium sulfate, followed by distilling-off of the solvent and purification by thin layer chromatography with benzene as the developer to obtain 205 mg of ethyl p-(3-trifluoromethylnonyloxy)benzoate (yield: 60.5%).
WORKUP
后处理
- distillationwas distilled off under a reduced pressure, and water
- additionwas added
- extractionfollowed by extraction with methylene chloride
- dry with materialThe methylene chloride solution was dried with magnesium sulfate
- distillationfollowed by distilling-off of the solvent and purification by thin layer chromatography with benzene as the developer