HRID1867410

反应详情

EQUATION

反应方程式

HRID 1867410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A solution of 0.50 g (1.11 mmol) of crude methanesulfonic acid 3-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-yl}-propyl ester in 20 ml of 2-butanone was treated with 0.33 g (2.23 mmol) of sodium iodide and stirred at 95° C. for 30 min. The reaction was cooled, evaporated, suspended in 60 ml dichloromethane/Et2O (1:3), filtered and the organic solvent discarded. The residue was then washed again with dichloromethane to give after evaporation 0.27 g (51%) of the title compound as white solid. MS: 481.0 (MH+, 2Cl).

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. customevaporated
  3. filtrationfiltered
  4. washThe residue was then washed again with dichloromethane
  5. customto give
  6. customafter evaporation 0.27 g (51%) of the title compound as white solid