HRID1375683

反应详情

EQUATION

反应方程式

HRID 1375683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl-3-iodobenzoate (25.4 g, 92.0 mmol) was dissolved in THF (60 mL) and cooled to 0° C. followed by the addition of KOt-Bu (20.6 g, 184 mmol). The mixture was stirred for 15 minutes followed by the addition of ethyl acetate (8.91 g, 101 mmol). The mixture was warmed to ambient temperature, stirred for 2 hours, diluted with aqueous HCl (10%, 200 mL) and extracted with ethyl acetate (2×150 mL). The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo to provide the titled compound (29.3 g, 100%).

WORKUP

后处理

  1. temperatureThe mixture was warmed to ambient temperature
  2. stirringstirred for 2 hours
  3. extractionextracted with ethyl acetate (2×150 mL)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo