[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1)[C:7]([NH2:9])=O)([O-:3])=[O:2].CCN(CC)CC.FC(F)(F)C(OC(=O)C(F)(F)F)=O.CC(=O)OCC>C(Cl)Cl>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:14])([F:15])[F:16])[CH:12]=1)[C:7]#[N:9])([O-:3])=[O:2]To a mixture of 3-nitro-5-(trifluoromethyl)benzamide (1.5 g, 6.41 mmol) in DCM (20 mL) were added Et3N (1.314 mL, 9.61 mmol) and trifluoroacetic anhydride (1.357 mL, 9.61 mmol) at 20° C. The mixture was stirred at 20° C. for 2 h. TLC (PE/EA=3:1, Rf=0.6) showed the reaction was finished. The reaction was concentrated to give crude product, which was purified by column chromatography (PE/EA=3:1, Rf=0.6) to give 3-nitro-5-(trifluoromethyl)benzonitrile (1.2 g, 5.14 mmol, 80% yield): 1H NMR (400 MHz, CDCl3-d) δ 8.71 (s, 2H), 8.24 (s, 1H).
불러오는 중…
