6-硝基喹哪啶的合成工艺改进

Process Improvement on the Synthesis of 6-Nitrylquinaldine

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:28.92 mmol,甲苯10 mL,混酸45.5 mL[V(AcOH)∶V(HCl)=1∶90],n(2)∶n(I2/KI)=1∶1,于100℃反应4 h,收率达93.1%。1的结构经1HNMR,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.