HRID18696

反应详情

EQUATION

反应方程式

HRID 18696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 17 (9 g, 0.021 mol), iron (3.65 g, 0.065 mol), and ammonium chloride (2.33 g, 0.043 mol) in isopropanol (200 ml)-water (50 ml) was stirred at 100° C. for 4 h. After cooling, the reaction mixture was filtrated and extracted with CH2Cl2. The combined organic layer was dried by MgSO4 and evaporated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3) to afford compound 18, yield 89%.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtrated
  3. extractionextracted with CH2Cl2
  4. dry with materialThe combined organic layer was dried by MgSO4
  5. customevaporated
  6. customto give a residue that
  7. customwas purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3)