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通过Suzuki-Miyaura偶联反应,以4-氯苯硼酸与2,3-二氯-1-溴苯为原料,以碳酸钾作为碱,分别在Pd(PPh_3)_4和Pd/C催化下,高效合成2,3,4’-三氯联苯,两种催化剂反应条件下产率均达到了95%.涉及Pd(PPh_3)_4催化的反应要求惰性气体反应氛围,且需在80oC下反应12 h.而无配体Pd/C催化的反应则在空气或者氧气氛围下反应加快,室温下30 min后反应产率即可达到95%.有关催化剂回收方面,Pd(PPh_3)_4对空气敏感,反应结束后未能回收,而无配体的Pd/C催化剂可循环使用5次以上且几无活性损失.与传统的含配体的Pd催化剂比较,无配体Pd/C催化在经济、环保以及实验操作方面表现出巨大的优势.
By Suzuki-Miyaura coupling reaction, 4-chlorobenzeneboronic acid and 2,3-dichloro-1-bromobenzene as raw materials, potassium carbonate as a base, respectively, Pd (PPh_3) _4 and Pd / C catalyst, efficient Synthesis of 2,3,4’-trichlorobiphenyl, the yield of both catalysts reached 95% .Reaction involving Pd (PPh_3) _4 reaction requires inert gas reaction atmosphere, and need to react at 80oC for 12 h Pd (PPh_3) _4 was sensitive to air, and the reaction rate was 95% after 30 min at room temperature.For the catalyst recovery, Pd (PPh_3) _4 was sensitive to air and the reaction The Pd / C catalyst without ligand can be reused for more than 5 times and with few loss of activity after the reaction.Compared with the traditional ligand-containing Pd catalyst, the ligand-free Pd / C catalyst has the advantages of economy, environmental protection and Experimental operation showed great advantages.