HRID1861951

反应详情

EQUATION

反应方程式

HRID 1861951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the compound (43.5 mg) obtained in Example 40 in acetonitrile (5 ml), a solution of hydrogen chloride in 1,4-dioxane (4N, 0.1 ml) and ethyl iodide (50 mg) were added and heated under reflux for 5 h. The reaction mixture was concentrated under reduced pressure and the resulting residue was purified by basic silica gel column chromatography (eluent, methylene chloride methanol=5:1) to give 9.2 mg of the titled compound (yield, 19%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 5 h
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe resulting residue was purified by basic silica gel column chromatography (eluent, methylene chloride methanol=5:1)