The Synthesis And Chromatographic Separation Of Calix [4] Arene Derivatives

Along with life sciences materials science and analysis scientific progress's needy, more and more scholar pay attention to the calixarenes the third generation superamolecular. And its application have been developed rapidly in recent year. For example, It have been applied in the fields of noble metal extraction, superamolecular catalysis, molecular self-assembly,ion, molecular recognition, drug development, chromatogram and so on. And it has been widely studied used as the mobile phase additive, bonded stationary and separation in the field of chromatogram. The paper mainly includes synthesis, chromatographic separation and ESI-MS fragmentation regularity of calixarene derivatives. In detail,it consists of three aspect contents as follow:1.p-tert-butylcalix[4]arene,25-Mono-(ethoxycarbonylmethoxy)-5,11,17,23-tert-buty lcalix[4]arene,25-Mono-(ammoniapropylammoniacarbonylmethoxy)-5,11,17,23-tert-butylcalix[4]arene, calix[4]arene,25-Mono-(ethoxycarbonylmethoxy)-calix[4]arene, 25,26,27,28-(tetraethoxy)-calix[4]arene,5,17-Diformyl-25,26,27,28-(tetraethoxy)-cali x[4]arene were synthesised and charecterized by IR,'HNMR and MS.The purities reach 87%-96.12% by High Performance Liquid Chromatography.2.Three groups calixarene mixture's chromatographic separation have been researched on the Agilent C-18 column, thermo C-18 column, the Agilent NH2 column, and received better result. By optimized chromatograph condition, they have a better separation and peak.3.Based on the rearch of ESI-MS fragmentation regularity with calix[4]arene and derivatives, we have found if having tert-butyl either no or few ethoxycarbonylmethoxy, the tert-butyl, next removeing ethoxycarbonylmethoxy were first removed; while not having tert-butyl, only the lower groups were removed.