N,N’-二(4-硝基苯)脲合成研究

Study on the Synthesis of N,N'-Bis(4-nitropheoyl)urea

以N,N二甲基甲酰胺为溶剂,由对硝基苯胺与尿素在回流温度反应得到N,N’二(4硝基苯)脲,纯度经液相色谱检测大于98.00%,收率达80.30%。反应原料配比经过实验优化,确定了最佳原料配比∶n(对硝基苯胺)∶n(尿素)∶n(浓盐酸)=1.00∶1.00∶1.25(摩尔比),最佳反应时间为每41.4g(0.3mol)对硝基苯胺原料回流温度反应5.0h(分批加入尿素需要1.0h)。

N,N'-Bis(4-nitrophenyl)urea was prepared by reacting p-nitroaniline with urea in the presence of DMF as solvent at refluxing temperature. The prepared product was analyzed by liquid chromatography. The purity of the product was above 98.00% and the yield was 80.30%. The optimal ratio of the reactants was p-nitroaniline: urea: concentrated hydrochloric acid=1.00∶1.00∶1.25, and the optimal reaction time was 5 h for 41.4 g(0.3 mol) p-nitroaniline under reflux temperature(adding the urea in batches within 1.0 h).