HRID18696
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- filtrationthe reaction mixture was filtrated
- extractionextracted with CH2Cl2
- dry with materialThe combined organic layer was dried by MgSO4
- customevaporated
- customto give a residue that
- customwas purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3)