反应详情

Under an argon atmosphere, 22.2 g of phenanthrene-2-boronic acid, 28.3 g of 4-bromoiodobenzene, 2.31 g of tetrakis(triphenyl phosphine) palladium(0), 400 mL of toluene, and 200 mL of a 2-M aqueous solution of sodium carbonate were loaded, and then the mixture was stirred for 8 hours under reflux. After having been cooled to room temperature, the reaction solution was extracted with toluene. The water layer was removed, and the organic layer was sequentially washed with water and a saturated salt solution, and was then dried with magnesium sulfate. After magnesium sulfate had been separated by filtration, the organic layer was concentrated. The residue was purified by silica gel column chromatography. Thus, 30.3 g of 10-(3-bromophenyl)benzo[c]phenanthrene were obtained (91%).

1. temperatureunder reflux
2. extractionthe reaction solution was extracted with toluene
3. customThe water layer was removed
4. washthe organic layer was sequentially washed with water
5. dry with materiala saturated salt solution, and was then dried with magnesium sulfate
6. customAfter magnesium sulfate had been separated by filtration
7. concentrationthe organic layer was concentrated
8. customThe residue was purified by silica gel column chromatography