Boron tribromide → HCID 135430634、化合物
反応式
B(Br)(Br)Br.[Cl:5][C:6]1[CH:11]=[C:10]([O:12]C)[CH:9]=[CH:8][C:7]=1[C:14]1[N:18]([CH3:19])[C:17]([C:20]23[CH2:27][CH2:26][C:23]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])([CH2:24][CH2:25]2)[CH2:22][CH2:21]3)=[N:16][N:15]=1>C(Cl)Cl>[Cl:5][C:6]1[CH:11]=[C:10]([OH:12])[CH:9]=[CH:8][C:7]=1[C:14]1[N:18]([CH3:19])[C:17]([C:20]23[CH2:27][CH2:26][C:23]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])([CH2:24][CH2:25]2)[CH2:22][CH2:21]3)=[N:16][N:15]=1参加物
4
実験手順
Boron tribromide (135 μL, 1.43 mmol) was added dropwise to a solution of 3-(2-chloro-4-methoxyphenyl)-4-methyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)4H-1,2,4-triazole (3-F) (287 mg, 0.714 mmol) in methylene chloride (5 mL) at 0° C. The mixture was stirred at room temperature for 2.5 h. The solution was washed with water, 10% NaHCO3, dried (MgSO4) and concentrated in vacuo and the residue purified by column chromatography (silica gel, 5% MeOH/methylene chloride) to provide 3-chloro-4-[4-methyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)--4H-1,2,4-triazol-3-yl]phenol (3-G). Mass spectrum: 388 (M+1); 1H NMR (500 MHz, CDCl3): δ 0.93 (t, 3H); 1.26 (m, 8H); 1.56 (m, 6H); 2.13 (m, 6H); 3.58 (s, 3H); 6.69 (dd, 1H); 6.92 (d, 1H); 7.09 (d 1H) ppm.