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研究了空气下无配体Pd(OAc)2在弱碱碳酸钾存在下催化二苯胺和溴代芳烃的C—N偶联合成三苯胺类化合物.与传统合成方法相比,该反应可以在无配体存在下在空气和温和的条件下进行,即,无需无水无氧操作条件,操作特别方便.催化剂用量、碱、溶剂、反应温度、反应时间等因素对反应的影响均做了考察.优化的反应条件是:在Pd(OAc)2(3 mol%)和K2CO3(1.5 equiv.)存在下,二苯胺和溴代芳烃在DMSO中在空气下在90℃加热24 h.溴代芳烃上的吸电子基团和二苯胺上的给电子基团有利于该偶联反应的进行,其中4-硝基三苯胺的产率高达93%.
In the presence of weak base potassium carbonate, Pd (OAc) 2, which catalyzes the C-N coupling of diphenylamine and brominated aromatics, to synthesize triphenylamines was studied in air. Compared with the traditional synthesis method, Ligands are carried out under air and under mild conditions, ie without the need of anhydrous and anaerobic operating conditions, the operation is particularly convenient.The effects of the amount of catalyst, base, solvent, reaction temperature and reaction time on the reaction are examined. The optimized reaction conditions were: Diphenylamine and bromoareromatics were heated in DMSO at 90 ° C for 24 h in the presence of Pd (OAc) 2 (3 mol%) and K2CO3 (1.5 equiv.) Of the electron-withdrawing group and the electron-donating group on the diphenylamine favored the coupling reaction, in which the yield of 4-nitrotriphenylamine was as high as 93%.