以I2/KI为氧化剂,甲苯为乳化剂,对硝基苯胺(2)和巴豆醛(3)经环合反应合成了6-硝基喹哪啶(1)。最佳反应条件为:28.92mmol,甲苯10mL,混酸45.5mL[V(AcOH):V(HCl)=1:90],n(2):n(12/KI)=1:1,于100℃反应4h,收率达93.1%。1的结构经1^H NMR,IR和元素分析表征。
6-Nitrylquinaldine( 1 ) was synthesized by cyclization of p-nitroaniline(2) with crotonalde- hyde(3) using I2/KI as the oxidant and toluene as the emulsifier. The structure was characterized by 1^ H NMR, IR and elemental analysis. The optimum reaction conditions at 100 ℃ for 4 h were as follows: 2 was 8.92 mmol; toluene was 10 mL; mixed acid[ V(AcOH) : V(HCl) = 1:90] was 45.5 mL; n(2) : n(I2/KI) = 1 : 1. The yield of 1 can reach 93.1% under the conditions.