【摘要】 以4-羟基-4′-氰基联苯(Ⅰ)为原料,在碳酸钾(水和乙醇作溶剂)溶液中与1,6-二溴己烷反应得到4-(6-溴己氧基)-4′-氰基联苯(Ⅱ),然后经过Gabriel反应、肼解反应制得4-(6-氨基己氧基)-4′-氰基联苯(Ⅳ)。与国外相似结构的合成工作相比,简化了反应步骤,且总收率由文献[2]的27.8%提高到55.2%。用IR、1HNMR和元素分析确证了目标产物的化学结构;经DSC测试,其液晶相转变温度为:Tm(熔点)83℃,Ti(清亮点)104℃。为了应用和贮存将其转变为相应的盐酸盐。更多还原

【Abstract】 4-（6-Aminohexyloxy）-4′-cyanobiphenyl（Ⅳ） was synthesized from 4-hydroxy-4′-cyanobiphenyl（Ⅰ） in three steps.Firstly,Ⅰ etherified with 1,6-dibromohexane to form 4-（6-bromohexyloxy）-4′-cyanobiphenyl（Ⅱ） in the presence of potassium carbonate.Then Ⅱ reacted with potassium phthalimide to give 4-（6-phthalimidohexyloxy）-4′-cyanobiphenyl（Ⅲ）.Finally,Ⅳ was obtained by hydrazinolysis of Ⅲ.The total yield reached as high as 55.2% compared with 27.8% in the literature^[2],at the same time the procedure was simplified.Structures of the target product（Ⅳ）and intermediates（Ⅱ,Ⅲ） were confirmed by IR,¹HNMR and elementary analysis.Melting point and clearing point of Ⅳ were 87 ℃ and 104 ℃ respectively by DSC.Compound Ⅳ reacted with dry HCl to give the corresponding salt for application and conservation.更多还原