Jozef Hodyl PhD Thesis - Theses - Flinders University

GPS, 33, linker material with an excess of the macrocycle 46, in dry toluene, or dryacetonitrile for 47 and 48, for 2 days at 60 o C followed by filtration and washing withtoluene for 46, or acetonitrile for 47, and 48, followed by Soxhlet extraction withmethanol as shown in Scheme 4.5.Scheme 4.5Synthesis of the silica attached macrocyclic ligands, Si-GPS-Trac, 43, Si-GPS-DiPTrac, 44, and Si-GPS-TriPTrac, 45.The silica materials Si-GPS-Trac, 43, Si-GPS-DiPTrac, 44, and Si-GPS-TripPTrac,45, were dried in vacuo and kept in a desiccator. Synthesis of the immobilisedmacrocyclic adducts, Si-GPDMS-Trac, 86, Si-GPS-Trac 230-400 , 87, and MCM-41-GPS-Trac, 88, and endcapped receptor material Si-GPS-Trac(EC), 89, followedprocedures identical with those used for the preparation of Si-GPS-Trac, 43. Thesynthesis of the endcapped material is depicted in Scheme 4.6.46 89Figure 4.6 Synthesis of the endcapped silica immobilised macrocyclic receptor ligand, 89.76