HRID1916573
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
- 110 °C
PROCEDURE
实验过程
652 mg (2.00 mmol) caesium carbonate, 36 mg (0.20 mmol) 1,10-phenanthroline and 19 mg (0.10 mmol) CuI are added to a solution of 289 mg (1.00 mmol) 1-bromo-4-iodobenzene and 0.27 mL (2.00 mmol) N-ethyl-3-hydroxypiperidine in 1.0 mL toluene. The reaction mixture is stirred for 36 h at 110° C. and then combined with 10 mL water and 10 mL EtOAc. After filtration the aqueous phase is extracted with 10 mL EtOAc and the combined organic extracts are washed with saturated NaCl solution and dried over Na2SO4. The solvent is eliminated i.vac. and further purification is carried out by column chromatography on silica gel (EtOAc).
WORKUP
后处理
- filtrationAfter filtration the aqueous phase
- extractionis extracted with 10 mL EtOAc
- washthe combined organic extracts are washed with saturated NaCl solution
- dry with materialdried over Na2SO4
- customand further purification