反应详情

Under an argon atmosphere, 3.26 g of the benzo[c]phenanthrene-5-boronic acid obtained, 2.83 g of 3-bromoiodobenzene, 0.231 g of tetrakis(triphenylphosphine)palladium(0), 40 mL of toluene and 20 mL of a 2M aqueous solution of sodium carbonate were placed in a flask. The resultant was refluxed with stirring for 8 hours. After cooling to room temperature, the reaction solution was extracted with toluene. An aqueous phase was removed and an organic phase which had been separated was washed with water and saturated brine sequentially, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The resulting residue was purified by means of silica gel column chromatography, whereby 3.64 g (yield: 95%) of 10-(3-bromophenyl)benzo[c]phenanthrene was obtained.

1. temperatureThe resultant was refluxed
2. extractionthe reaction solution was extracted with toluene
3. customAn aqueous phase was removed
4. customan organic phase which had been separated
5. washwas washed with water and saturated brine sequentially
6. dry with materialdried with magnesium sulfate
7. filtrationAfter the magnesium sulfate was filtered out
8. concentrationthe organic phase was concentrated
9. customThe resulting residue was purified by means of silica gel column chromatography