HRID732535

反应详情

EQUATION

反应方程式

HRID 732535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Mix 5-iodo-N-methyl-N-propyl-isophthalamic acid methyl ester (220 mg, 0.61 mmol), 2-pyrrolidone (56 μL, 0.73 mmol), ethane-1,2-diamine (4 μL, 0.061 mmol), cesium carbonate (398 mg, 1.22) and copper (I) iodide (12 mg, 0.061 mmol) in 1,4-dioxane (4 mL). Heat the mixture to 110° C. for 1 h then stir at room temperature overnight. Dilute with dichloromethane and filter through a filtering agent. Concentrate and purify (silica gel chromatography, eluting with ethyl acetate and hexanes) to give the title compound (100 mg, 52%).

WORKUP

后处理

  1. filtrationfilter through a filtering agent
  2. concentrationConcentrate
  3. custompurify
  4. wash(silica gel chromatography, eluting with ethyl acetate and hexanes)