Abstract
Tritium labelled compounds are widely used in the physical and life sciences. The preparation of such compounds is a very important area of chemistry. Although the methods are, on the whole, fairly simple and straightforward, there is still a need for improvement. The same applies as far as the analysis of the tritium distribution is concerned. High resolution 3H NMR spectroscopy of solutions is now a well established technique. However many compounds exist as solids which are either insoluble or sparingly soluble in organic solvents, consequently there is a need to develop high resolution 3H NMR spectroscopy of solids. The thesis therefore consists of four chapters. The first is a review dealing with the properties of tritium, the various labelling methods and tritium nuclear magnetic resonance spectroscopy. In the second chapter an account is given of the way in which complex metal tritides and tritiated methyl iodide, an important reagent which enables one to introduce three tritium atoms in a single step and therefore obtain products of very high specific activity, are prepared. In the third chapter an account is given of the synthesis and attempted tritiation of two potential 5-HT re-uptake inhibitors, prior to their use in biological studies. Whilst the synthesis of the two compounds N-[[[l-[(l-bromo-2-naphthalenyl)methyl]-4-piperidinyl]amino]carbonyl]-3-pyridinecarboxamide, and N-[[[l-[(l-bromo-6-fluoro-2-naphthalenyl)methyl] -4-piperidinyl]amino]carbonyl]-3-pyridinecarboxamide, was successful the tritiation procedure led to unforseen difficulties. Finally in the fourth chapter solid state tritium NMR spectroscopy, using a magic angle accessory, was developed and used in the analysis of several tritiated compounds.