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(Cont.) Chapter Two: N-(2-mercaptoethyl)picolylamine (MEPAH) was studied as a potentially biologically relevant ligand for the 'fac-[M(CO)3]+" core (M = Re, 99Tc, 99mTc). To this end, the complex Re(CO)3(MEPA) was synthesized. The reaction of MEPAH with fac-[Re(CO)3(MeCN)3]+ took place over the course of seconds, showing the high affinity possessed by this ligand for the "fac-[Re(CO)3]+" core. A single crystal X-ray diffraction study was performed, confirming the nature of Re(CO)3(MEPA), a rare mononuclear rhenium(I) thiolate complex. Exploration into derivatization of the ligand backbone has afforded the analogous N-ethyl complex, Re(CO)3(MEPA-NEt). Further work has given rhenium complexes of bioconjugated ligands, whereby biologically active molecules have been tethered to the ligand framework. The high affinity of the ligand for the metal, coupled with the ease of its derivatization, implies that this ligand system is promising for the purposes of 99mTc radiopharmaceutical development. Chapter Three: The bioevaluation of 99mTc complexes of derivatives of MEPAH is described. Complexes analogous to the tricarbonylrhenium(I) complexes described in Chapter 2 were synthesized and characterized by HPLC. After confirmation of the composition of these 99mTc complexes, in vitro and in vivo studies were performed. These compounds of the "fac-[99mTc(CO)3]+' core, containing the biologically active molecules morpholine and nornicotine, were evaluated for uptake by melanoma and brain tissue, respectively, in mice.