New methods for the construction of fluorinated cyclic amines and amides

In recent years, photoredox catalysis has emerged as a powerful tool for the synthesis of complex building blocks. Fluorine-containing saturated nitrogen heterocycles are desirable structures in medicinal and biological chemistry, as the incorporation of fluorine can be used to influence key propert...

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Main Author: Charlesworth, Natalie
Format: Thesis (University of Nottingham only)
Language:English
Published: 2022
Subjects:
Online Access:https://eprints.nottingham.ac.uk/67503/
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author Charlesworth, Natalie
author_facet Charlesworth, Natalie
author_sort Charlesworth, Natalie
building Nottingham Research Data Repository
collection Online Access
description In recent years, photoredox catalysis has emerged as a powerful tool for the synthesis of complex building blocks. Fluorine-containing saturated nitrogen heterocycles are desirable structures in medicinal and biological chemistry, as the incorporation of fluorine can be used to influence key properties of a compound such as conformation, basicity and bioavailability. This thesis explores the utilisation of a photoredox-catalysed cyclisation/hydrogen atom transfer reaction of bromodifluoroethylamines, using a modular, two-step approach. The first chapter provides an introduction to photoredox catalysis, notable developments in the area and relevant examples from the literature of photoredox-mediated radical cyclisation reactions. Following this, the importance of fluorination in drug discovery is discussed, along with traditional methods for the introduction of the geminal difluoro- group. The second chapter describes a photoredox radical cyclisation protocol using bromodifluoroethylamines, which are prepared through a three-component coupling. The reaction is applicable to a wide range of alkenyl- and alkynyl amines, and the utility of the products are demonstrated. Mechanistic investigations established the role of the tertiary amine base and the additional hydrogen-atom donor in the reactions. The success of the described approach relies on the strongly electron-withdrawing nature of fluorine, which prevents oxidation of the amine substrates and products under the reaction conditions. This eliminates the need for electron-withdrawing protecting groups on nitrogen and promotes cyclisation. The third chapter builds on the developed photoredox catalysed cyclisation for the mild and efficient synthesis of γ- and δ-lactams. The protocol is applicable to a range of amide substrates, and a mechanism for the reaction is proposed, supported by computational calculations.
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spelling nottingham-675032022-08-02T04:40:08Z https://eprints.nottingham.ac.uk/67503/ New methods for the construction of fluorinated cyclic amines and amides Charlesworth, Natalie In recent years, photoredox catalysis has emerged as a powerful tool for the synthesis of complex building blocks. Fluorine-containing saturated nitrogen heterocycles are desirable structures in medicinal and biological chemistry, as the incorporation of fluorine can be used to influence key properties of a compound such as conformation, basicity and bioavailability. This thesis explores the utilisation of a photoredox-catalysed cyclisation/hydrogen atom transfer reaction of bromodifluoroethylamines, using a modular, two-step approach. The first chapter provides an introduction to photoredox catalysis, notable developments in the area and relevant examples from the literature of photoredox-mediated radical cyclisation reactions. Following this, the importance of fluorination in drug discovery is discussed, along with traditional methods for the introduction of the geminal difluoro- group. The second chapter describes a photoredox radical cyclisation protocol using bromodifluoroethylamines, which are prepared through a three-component coupling. The reaction is applicable to a wide range of alkenyl- and alkynyl amines, and the utility of the products are demonstrated. Mechanistic investigations established the role of the tertiary amine base and the additional hydrogen-atom donor in the reactions. The success of the described approach relies on the strongly electron-withdrawing nature of fluorine, which prevents oxidation of the amine substrates and products under the reaction conditions. This eliminates the need for electron-withdrawing protecting groups on nitrogen and promotes cyclisation. The third chapter builds on the developed photoredox catalysed cyclisation for the mild and efficient synthesis of γ- and δ-lactams. The protocol is applicable to a range of amide substrates, and a mechanism for the reaction is proposed, supported by computational calculations. 2022-08-02 Thesis (University of Nottingham only) NonPeerReviewed application/pdf en cc_by https://eprints.nottingham.ac.uk/67503/1/Natalie%20Charlesworth%20Thesis%20Post-Viva%20Corrections.pdf Charlesworth, Natalie (2022) New methods for the construction of fluorinated cyclic amines and amides. PhD thesis, University of Nottingham. Fluorinated cyclic amines Amides
spellingShingle Fluorinated cyclic amines
Amides
Charlesworth, Natalie
New methods for the construction of fluorinated cyclic amines and amides
title New methods for the construction of fluorinated cyclic amines and amides
title_full New methods for the construction of fluorinated cyclic amines and amides
title_fullStr New methods for the construction of fluorinated cyclic amines and amides
title_full_unstemmed New methods for the construction of fluorinated cyclic amines and amides
title_short New methods for the construction of fluorinated cyclic amines and amides
title_sort new methods for the construction of fluorinated cyclic amines and amides
topic Fluorinated cyclic amines
Amides
url https://eprints.nottingham.ac.uk/67503/