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 an argon gas atmosphere, 39.25 g (177 mmol) of 9-phenanthreneboronic acid, 50.0 g (177 mmol) of 4-bromoiodobenzene, 4.10 g (3.54 mmol) of tetrakis(triphenylphosphine) palladium(0), 400 mL of toluene and 265 mL of 2M sodium carbonate solution were mixed, and stirred for 24 hours while being refluxed. After the reaction in the mixture was over, the mixture experienced filtration, through which aqueous phase thereof was eliminated. After organic phase thereof was cleansed by water and dried with magnesium sulfate, toluene was distilled away under reduced pressure. Residue thereof was refined by silica-gel column chromatography, such that 42.6 g of 9-(4-bromophenyl)phenanthrene was obtained with an yield of 72%.
WORKUP
后处理
- temperaturewhile being refluxed
- customAfter the reaction in the mixture
- filtrationfiltration
- dry with materialdried with magnesium sulfate, toluene
- distillationwas distilled away under reduced pressure
- customwas obtained with an yield of 72%