杯芳烴衍生物论文生物的合成及25,27-二(3-甲基噻二唑基硫代乙氧基)杯芳烃固定相的色谱性能研究.docVIP

杯[4]芳烃衍生物论文：杯[4]芳烃衍生物的合成及25，27-二（3-甲基噻二唑基硫代乙氧基）杯[4]芳烃固定相的色谱性能研究 【中文摘要】杯芳烃固定相是杯芳烃化学中最令人关注的研究热点之一,自二十世纪四十年代Zinke小组制备了杯芳烃以来,越来越多的杯芳烃衍生物,如：杯芳冠醚、手性杯芳烃、杂原子杯芳烃、杯芳烃聚合物等被合成出来。至今,关于杯芳烃的研究已趋于成熟,在多个领域中得到了广泛应用。本论文合成了一些杯芳烃衍生物,并优化了其合成过程,效果令人满意。从中选择了25,27-二(3-甲基噻二唑基硫代乙氧基)杯芳烃与硅胶键合,合成了25,27-二(3-甲基噻二唑基硫代乙氧基)杯芳烃固定相,对其进行了表征,并将其应用于高效液相色谱性能研究。论文主要内容包括以下三个方面：1.合成了一系列的杯芳烃衍生物,如：25,27-二(溴乙氧基)杯芳烃、25,27-二(a-甲基苄胺基乙氧基)杯芳烃、25-(乙氧羰基甲氧基)杯芳烃、25,27-二(乙氧羰基甲氧基)杯芳烃、25-(氨丙基氨羰基甲氧基)杯芳烃、1,3-杯芳烃、1,2-杯芳烃-冠-4和25,27-二(3-甲基噻二唑基硫代乙氧基)杯芳烃。并用质谱、核磁共振、色谱分离等技术对杯芳烃衍生物进行了表征,取得满意结果。2.合成了25,27-二(3-甲基噻二唑基硫代乙氧基)杯芳烃固定相,并用红外、热重分析、元素分析等方法对其进行了表征。其化学性质和热稳定性良好,键合量为0.052 mmol/g,柱效为9073块/米,连续使用10个月,柱效变化小于9%,保留时间变化小于3%。3.在杯芳烃色谱柱上,对苯胺衍生物、多环芳烃、苯甲酸衍生物等一系列分析靶物进行了分离,并与商用C18进行了对比研究,发现杯芳烃固定相除了具有C18的疏水作用外,还具有多种作用机制,如：p-p作用、氢键作用和包结作用等。 【英文摘要】The calixarene stationary phase is one of the most interested fields in calixarene chemistry. Since Zinke discovered calixarene in 1940s, the synthesis of calixarene was improved continuously and more calixarene derivatives, like calixcrowns, chiral calixarenes, heteroatom calixarenes and calix-polymers were obtained. And they were widely used in many fields now. In this thesis studied, the synthesis of some calix[4]arene derivatives were optimized, and acquired good results. The calix[4]arene stationary phase with diazole group was bonded on silica gel and applied on research of the chromatographic performance. Three contents were studied in this article:1. Some p-tert-butyl calix[4]arene derivatives were synthesized:25,27-bis(bromoe-thyoxyl)-calix[4]arene,25,27-bis(a-methylbenzylamine ethyoxyl)-calix[4]arene,25-(etho-xycarbonyl methoxyl)-calix[4]arene,25,27-bis(ethoxycarbonyl methoxyl)-calix[4]arene,25-(Aminopropyl aminocarbonyl methoxyl)-calix[4]arene, 1,3-[propyl-bis(aminocarbonyl meth-oxyl)]-calix[4]arene, calix[4]arene-1,2-crown-4 and 25,27-bis-(3-methylthiadiazole thioeth-yoxyl)-calix[4]arene. And characterized by MS,’H NMR and HPLC. T