HRID225717

反应详情

EQUATION

反应方程式

HRID 225717 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To 30.7 mmol 2-Iodo-5-methanesulfonyl-benzoic acid in 250 ml THF was added 33.7 mmol CDI and the mixture was heated at 70° C. for 1 h. Methanol (12.4 ml) was then added and the mixture was heated at 70° C. for a further 1 h. The mixture was then cooled to room temperature and concentrated in vacuo. The residue was chromatographed over SiO2 (ethyl acetate/dichloromethane 4:1) to afford the title compound (86%) as a white crystalline solid.

WORKUP

后处理

  1. temperaturethe mixture was heated at 70° C. for a further 1 h
  2. temperatureThe mixture was then cooled to room temperature
  3. concentrationconcentrated in vacuo
  4. customThe residue was chromatographed over SiO2 (ethyl acetate/dichloromethane 4:1)