反应详情

温度

50 °C

In a three-necked flask equipped with a condenser, a thermometer and a stirrer were placed 26.8 g of 6-bromo-2-naphthol, 4.6 g of tetrakistriphenylphosphinepalladium and 100 ml of toluene and the mixture was stirred at 50° C. When the solids nearly dissolved, a solution of 14.6 g of phenylboronic acid in 100 ml of ethanol was added and stirred. When the solutions mixed with each other, a solution of 30 g of sodium carbonate in 100 ml of water was added, the mixture was heated to the reflux temperature and stirred for 1 hour. Upon completion of the reaction, dilute hydrochloric acid was added until the aqueous layer became weakly acidic, the organic layer was recovered and the solvent was distilled off under reduced pressure. The crude product was recrystallized from 50 ml of toluene and the crystals collected by filtration were washed with toluene and dried at 80° C. under reduced pressure to give 11.9 g of 6-phenyl-2-naphthol. The unreacted 6-bromo-2-naphthol was not detected by HPLC.

1. customIn a three-necked flask equipped with a condenser
2. dissolutionWhen the solids nearly dissolved
3. stirringstirred
4. additionwas added
5. temperaturethe mixture was heated to the reflux temperature
6. stirringstirred for 1 hour
7. additionwas added until the aqueous layer
8. customthe organic layer was recovered
9. distillationthe solvent was distilled off under reduced pressure
10. customThe crude product was recrystallized from 50 ml of toluene
11. filtrationthe crystals collected by filtration
12. washwere washed with toluene
13. customdried at 80° C. under reduced pressure