间-乙酰氨基硝基苯与溴苯缩合反应的研究

间-乙酰氨基硝基苯与溴苯发生Ullmann缩合反应是制备3-硝基二苯胺最常用的方法。在氮气保护下,从反应时间、反应温度、催化剂以及它们的物料比方面对此反应作了研究。优惠反应条件为:反应时间24h,反应温度163℃,催化剂为铜粉,物料比n(间-乙酰氨基硝基苯)∶n(溴苯)=1∶1.5。在上述条件下N-乙酰基-3-硝基二苯胺的收率为98%。

Study on the Condensation of N-(3-Nitroph-enyl) Acetamide with Bromobenzene

3-Nitrodiphenylamine is generally synthesized by the Ullmann condensation of N-(3-nitrophenyl) acetamide with bromobenzene. The effects of the reaction time,the reaction temperature,kind of catalyst used,as well mole ratios between materials,were studied for the condensation. The optimal reaction condition was that reaction time was 24 h;reaction temperature was 163℃;the catalyst was powder of Cu,the mole ratio of N-(3-nitrophenyl)acetamide to bromobenzene was 1∶1.5.The yield of N-acetyl-3-nitrodiphenylamine was 98% under the optimal reaction condition.