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The search for radicals in unexpected places

  • Kenneth Clark

Student thesis: Doctoral Thesis

Abstract

In the last century, many literature reports discuss the electron-transfer from simple alkoxides, in particular NaOtBu and KOtBu, to aryl halides. These reports are controversial with many providing evidence on the contrary. This thesis will initial focus on explaining the role of these alkoxides in the transformations and reports on mechanistic investigations. Heating 9-bromoanthracene I with KOtBu yields 6 principal products (II-VII), all of which can be explained through radical chemistry (Scheme 1). Additionally, methylated compounds (V, VIII-X) are formed which are shown to result from the addition of methyl radicals (formed after electron transfer from tert-butoxide and subsequent collapse of the tert-butoxyl radical) to arenes. These are the first examples of alkylated arenes resulting from the collapse of alkoxyl radicals in the BHAS reaction and is undisputable evidence of electron transfer from KOtBu. Characterisation of the BHAS reaction with iodoarene XI was then significantly studied and was shown to provide important information about mechanism (Scheme 2). The experiments additionally demonstrated that substrate XI could be utilised as a stringent assay for xylyl radicals. Finally, determination of radical intermediates in organometallic reactions (e.g. Ni, Pd, Cu) can be challenging. A strict assay that allows for clear identification of aryl radical intermediates is required. Using substrate XI as an assay, organopalladium conditions that promote radical pathways were investigated and systems that direct to a radical route were disclosed (Scheme 3). [See thesis for schemes illustrations]
Date of Award20 Jan 2023
Original languageEnglish
Awarding Institution
  • University Of Strathclyde
SponsorsUniversity of Strathclyde
SupervisorJohn Murphy (Supervisor) & David Nelson (Supervisor)

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