HRID1661909
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
- 180 °C
PROCEDURE
实验过程
A mixture of 430 mg (1.07 mmol) 5-bromo-2-(4-isopropyl-phenyl)-7-methoxy-1-(2-methoxy-ethyl)-1H-benzoimidazole (example 22), 125 mg (1.07 mmol) zinc cyanide and 20 mg tetrakis(triphenylphosphine) palladium in 5 ml DMF is heated in a microwave oven for 75 min (180° C.). After that the reaction mixture is poured on water and extracted (3×) with ethyl acetate. The combined organic layers are washed with water (3×) and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue is purified by flash-chromatography on silica gel (hexane:EtOAc=3:1) to afford 250 mg of the title compound as a colorless solid.
WORKUP
后处理
- additionAfter that the reaction mixture is poured on water
- extractionextracted (3×) with ethyl acetate
- washThe combined organic layers are washed with water (3×) and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue is purified by flash-chromatography on silica gel (hexane:EtOAc=3:1)