HRID2073430

反应详情

EQUATION

反应方程式

HRID 2073430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. distillationwas distilled off under a reduced pressure, and water
  2. additionwas added
  3. extractionfollowed by extraction with methylene chloride
  4. dry with materialThe methylene chloride solution was dried with magnesium sulfate
  5. distillationfollowed by distilling-off of the solvent and purification by thin layer chromatography with benzene as the developer