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Title: Optimisation of catalytic systems using design of experiment methodologies
Author: McNamara, Catherine Anne
ISNI:       0000 0001 3388 586X
Awarding Body: University of Southampton
Current Institution: University of Southampton
Date of Award: 2004
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A Sharpless ligand with a novel triazene core was synthesised in two simple, high yielding steps from cheap, readily available starting materials. The ligand showed good selectivity in the asymmetric dihydroxylation of alkenes, and its optimisation was undertaken in collaboration with Dr D.C. Woods and Professor S.M. Lewis of Southampton University's Statistical Sciences Research Institute. Using a number of statistical designs and experimental methods, the results showed that the conditions reported and currently used were optimal. In the process of the investigation a greater understanding of the factors affecting the reaction was obtained. In a second example, C-C bond formation was optimised using a supported palladium catalyst. Four different sulfur containing pincer ligands were synthesized and attached to four different solid supports. Subsequent complexation with palladium gave 16 different polymer supported catalysts which were active catalysts in the Heck reaction.  The optimisation of this system with regards to both conversion and palladium leaching was undertaken using the experimental design software, MODDE which showed that solvent had the largest effect on both responses. The cHexyl thiol moiety was superior to its phenyl counterpart which is most commonly adopted. In the Heck reaction of 4-bromo acetophenone the conversion was improved from 30% with large observable leaching to 88% with no observable leaching varying 6 factors corresponding to 5760 possibilities.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available