HRID854493
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
PROCEDURE
实验过程
A slurry of 2.63 g (22.5 mmol) indole, 5.26 g (22.5 mmol) 4-iodoanisole, 0.43 g (3 mmol) CuBr and 4.14 g (30 mmol) K2CO3 in 60 ml anhydrous N-methylpyrrolidinone (NMP) was heated to reflux with stirring for 16 hr. The solution was allowed to cool and then poured into water and shaken with ethyl acetate. The entire biphasic system was filtered through a pad of Celite, the phases were separated, and the organic phase was dried over MgSO4 and concentrated. The crude product was chromatographed on silica (5–7% EtOAc-Hexane) to afford 3.53 g 1-(4-methoxyphenyl)-1H-indole as a colorless solid.
WORKUP
后处理
- temperatureto reflux
- temperatureto cool
- filtrationThe entire biphasic system was filtered through a pad of Celite
- customthe phases were separated
- dry with materialthe organic phase was dried over MgSO4
- concentrationconcentrated
- customThe crude product was chromatographed on silica (5–7% EtOAc-Hexane)