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
Under the atmosphere of argon, 230 g of 1,4-dibromonaphthalene, 121 g of 2-formylphenylboronic acid and 18.5 g of tetrakis(triphenylphosphine)palladium(0) were placed in a flask. To the resulting mixture, 2.4 L of dimethoxyethane (DME) and 1.2 L of an aqueous 2M sodium carbonate solution were added, followed by stirring under reflux for 8 hours. After cooling to the room temperature, an aqueous phase was removed, and an organic phase was washed with water and saturated saline, and dried with magnesium sulfate. After filtering off magnesium sulfate, the organic phase was concentrated. The residues were purified by silica gel column chromatography, whereby 170 g (yield 67%) of 1-bromo-4-(2-formylphenyl)naphthalene as an intended product was obtained.
WORKUP
后处理
- temperatureunder reflux for 8 hours
- customan aqueous phase was removed
- washan organic phase was washed with water and saturated saline
- dry with materialdried with magnesium sulfate
- filtrationAfter filtering off magnesium sulfate
- concentrationthe organic phase was concentrated