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二苯乙炔类化合物是高折射率向列相液晶材料的重要成份,其主要合成方法 Sonogashira偶联反应存在着合成路线较长、产率偏低等缺点,不利于工业化生产。基于Sonogashira偶联反应机理,简化二苯乙炔类液晶化合物的合成步骤,以期缩短合成路线,提高全合成产率。实验结果表明,当以取代溴苯为原料,将二苯乙炔类化合物的合成步骤简化成“二步”时,其全合成产率高达73.72%,比“一步法”提高40%左右,比“三步法”和“多步法”提高15%左右;缩短了合成路线,提高了合成效率;探索出最佳反应条件:以高沸点非质子氢试剂(如甲苯)为溶剂,KOH为碱性物质,DMAP为胺类物质,110℃下反应12 h。
Diphenyl acetylenes are important components of high refractive index nematic liquid crystal materials. The main synthesis methods of Sonogashira coupling reaction are long synthesis route, low yield and other disadvantages, which is not conducive to industrial production. Based on the Sonogashira coupling reaction mechanism, the synthesis steps of the benzenes are simplified in order to shorten the synthesis route and increase the total synthesis yield. The experimental results show that when the substituted bromobenzene is used as the raw material, the synthesis yield of the benzenes is reduced to 73.72%, which is 40% higher than that of “one-step method” About 15% higher than the “three-step method” and “multi-step method”; shorten the synthesis route and improve the synthesis efficiency; explore the best reaction conditions: high boiling point aprotic hydrogen reagent ) As solvent, KOH as basic material, DMAP as amines, reaction at 110 ℃ for 12 h.