【摘要】 报道了改进的二环己基并-18-冠-6(DCH-18-C-6)合成方法,并用该法实现了DCH-18-C-6的工业规模合成。对由二苯并-18-冠-6加氢合成DCH-18-C-6的反应中使用的Picher-钌催化剂进行了改性,用pH 3~5条件下新制备的Picher-钌催化剂,将反应温度提高并控制在130~140℃之间,可使氢化产率由文献报道的最高65%提高到85%以上,还显著提高了产物中DCH-18-C-6的立体异构体A(cis-syn-cis)含量。建立了用气相色谱法测定DCH-18-C-6异构体含量的方法,并用正庚烷进行结晶以实现A(cis-syn-cis)的提纯。更多还原

【Abstract】 An improved process for synthesis of dicyclohexyl-18crown-6(DCH-18-C-6) was reported,and the commercial-scale synthesis of DCH-18-C-6 was implemented.In the process of hydrogenation of dibenzo-18-crown-6 to form DCH-18-C-6,the modified Picher ruthenium catalyst was adopted.The catalyst was prepared in acidic condition at a pH value of 3～5 and used in-situ.In addition,the reaction temperature was strictly controlled within the range of 130～140 ℃.With these measures,the yield of hydrogenate was increased to more than 85%,which was apparently higher than the maximum reported yield 65%.Furthermore,the content of stereo-isomer of DCH-18-C-6,A(cis-syn-cis) was also increased up to 20%.The GC determination of the stereo-isomers was performed,and the stereo-isomer A(cis-syn-cis) was effectively purified by re-crystallization in n-heptane.更多还原