Triethyl Phosphate → 9H-Dibenzo[a,c]carbazole, 11-bromo-
반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]3[C:14]([C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=4[CH:21]=2)=[CH:13][CH:12]=[CH:11][CH:10]=3)=[C:4]([N+:22]([O-])=O)[CH:3]=1.P(OCC)(OCC)(OCC)=O>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[C:8]3[C:21]([NH:22][C:4]=2[CH:3]=1)=[C:20]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]1=[C:14]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=31참가 물질
3
실험 절차
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.