反应详情

A 250 mL round bottom flask was charged with 9-(4-bromo-2-nitrophenyl)phenanthrene (26.36 g, 69.69 mmol), and triethyl phosphate (84.84 mL, 487.86 mmol), and the mixture was heated under reflux at 160° C. to 165° C. for 14 hours. After the reaction was completed, the remaining triethyl phosphate was removed by vacuum distillation. The resultant product was diluted with a mixed solvent of MeOH:H2O=1:1, and the produced solid was filtered. The obtained solid was washed with a mixed solvent of MeOH:H2O=1:1, and petroleum ether. The solid was dissolved in methylene chloride, dried with MgSO4, and concentrated, and purified by silica gel column (petroleum ether:methylene chloride=2:1). Then, 14.96 g of a product (62%) was obtained.

1. temperaturethe mixture was heated
2. temperatureunder reflux at 160° C. to 165° C. for 14 hours
3. customthe remaining triethyl phosphate was removed by vacuum distillation
4. additionThe resultant product was diluted with a mixed solvent of MeOH
5. filtrationH2O=1:1, and the produced solid was filtered
6. washThe obtained solid was washed with a mixed solvent of MeOH
7. dissolutionThe solid was dissolved in methylene chloride
8. dry with materialdried with MgSO4
9. concentrationconcentrated
10. custompurified by silica gel column (petroleum ether:methylene chloride=2:1)