反应详情

In argon atmosphere, a mixture of 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 a 2 M sodium carbonate aqueous solution was refluxed under stirring for 24 h. After the reaction, the reaction mixture was filtered and the aqueous phase was removed. The organic phase was washed with water and dried over magnesium sulfate, and then the toluene was removed by distillation under reduced pressure. The residue was purified by silica gel chromatography to obtain 42.6 g (yield: 72%) of 9-(4-bromophenyl)phenanthrene.

1. temperaturewas refluxed
2. customAfter the reaction
3. filtrationthe reaction mixture was filtered
4. customthe aqueous phase was removed
5. washThe organic phase was washed with water
6. dry with materialdried over magnesium sulfate
7. customthe toluene was removed by distillation under reduced pressure
8. customThe residue was purified by silica gel chromatography