化学合成。
化学合成
合成路线 1(1. 合成:163444-17-5)
产率:97%
合成条件:With Iodine monochloride In methanol; dichloromethane at 0 - 20℃;
实验步骤:步骤2 2-碘-4-(三氟甲基)苯胺向500mL三颈圆底烧瓶中加入4-(三氟甲基)苯胺(22.5g,0.14mol)和MeOH(100mL)。 在0℃下向上述溶液中滴加IC1(25g,0.15mol)在CH 2 Cl 2(100mL)中的溶液。将得到的混合物在室温下搅拌1小时。 通过TLC监测反应进程(EtOAc /石油醚= 1:10,R f = 0.5)。 后处理:将混合物真空浓缩。 将残余物重新溶解在CH 2 Cl 2中,用水洗涤,用无水Na 2 SO 4干燥并真空浓缩,得到37.8g(97%)产物。 1H NMR(300MHz,CDCl3)δ:7.86(d,J = 1.2Hz,1H),7.36(dd,J = 8.4,1.8Hz,1H),6.73(d,J = 8.7Hz,1H),4.41( br,2H)。
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