| Summary: | <p>This thesis describes the development of two new rhodium-catalysed hydroacylation methods. The first involves a one-pot hydroacylation/thio-conjugate addition cascade towards the synthesis of fully saturated sulfur heterocycles. The second exploits novel β-sulfonyl aldehydes to access β-keto-sulfones and sulfonamides.</p>
<p><strong>Chapter 1</strong> delineates a literature review of the evolution of rhodium-catalysed hydroacylation, with focus on catalyst design and chelating groups that hinder decarbonylation. The use of hydroacylation in heterocycle synthesis is also briefly reviewed.</p>
<p><strong>Chapter 2</strong> documents the use of alkynes with pendant sulfur nucleophiles in a highly regioselective rhodium-catalysed hydroacylation reaction, delivering linear α,β-unsaturated enone intermediates. These adducts are further harnessed in intramolecular cyclisation reactions to access diversely substituted, saturated S-heterocycles, in a one-pot fashion.</p>
<p><strong>Chapter 3</strong> outlines initial attempts to develop a rhodium-catalysed hydroacylation methodology for the synthesis of β-keto-sulfones and sulfonamides. The work explores the construction of new β-sulfonyl aldehydes and their use in intermolecular hydroacylation.</p>
<p><strong>Chapter 4</strong> presents the conclusions from the research conducted and future work.</p>
<p><strong>Chapter 5</strong> details the experimental data and procedures.</p>
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