Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts

We disclose a novel synthetic method to access the homocubane ester 4a in 4 steps, in an overall yield comparable or superior to literature methods. The sequential transformations of a [6+2] cycloaddition, 4π electrocyclisation, followed by a dehydrogenation and [2+2] cycloaddition displays the rela...

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Main Author: Smithson, Jack
Format: Thesis (University of Nottingham only)
Language:English
Published: 2025
Subjects:
Online Access:https://eprints.nottingham.ac.uk/81034/
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author Smithson, Jack
author_facet Smithson, Jack
author_sort Smithson, Jack
building Nottingham Research Data Repository
collection Online Access
description We disclose a novel synthetic method to access the homocubane ester 4a in 4 steps, in an overall yield comparable or superior to literature methods. The sequential transformations of a [6+2] cycloaddition, 4π electrocyclisation, followed by a dehydrogenation and [2+2] cycloaddition displays the relatively simple route to access this challenging to make structure. We also inadvertently synthesised an interesting polycyclic structure we have tentatively assigned as formal [4+2] product 6. Herein, we report the development of a methodology for the regioselective 1,4-addition of propargyl boronates to a range of N-alkylated pyridinium, quinolinium, and pyrazinium salts, through gold-(I) mediated catalysis. A variety of functionality is tolerated under the mild reaction conditions, and an attempt to rationalise the mechanism has been realised with the assistance of DFT studies. Further potential chemical transformations have also been conducted, which, when combined with the work conducted in this study, pave the way for exploration into underdeveloped and diverse chemical space.
first_indexed 2025-11-14T21:05:05Z
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institution University of Nottingham Malaysia Campus
institution_category Local University
language English
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publishDate 2025
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spelling nottingham-810342025-07-30T04:40:18Z https://eprints.nottingham.ac.uk/81034/ Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts Smithson, Jack We disclose a novel synthetic method to access the homocubane ester 4a in 4 steps, in an overall yield comparable or superior to literature methods. The sequential transformations of a [6+2] cycloaddition, 4π electrocyclisation, followed by a dehydrogenation and [2+2] cycloaddition displays the relatively simple route to access this challenging to make structure. We also inadvertently synthesised an interesting polycyclic structure we have tentatively assigned as formal [4+2] product 6. Herein, we report the development of a methodology for the regioselective 1,4-addition of propargyl boronates to a range of N-alkylated pyridinium, quinolinium, and pyrazinium salts, through gold-(I) mediated catalysis. A variety of functionality is tolerated under the mild reaction conditions, and an attempt to rationalise the mechanism has been realised with the assistance of DFT studies. Further potential chemical transformations have also been conducted, which, when combined with the work conducted in this study, pave the way for exploration into underdeveloped and diverse chemical space. 2025-07-30 Thesis (University of Nottingham only) NonPeerReviewed application/pdf en cc_by https://eprints.nottingham.ac.uk/81034/1/Jack%20Smithson%20Thesis%20-%20Corrected.pdf Smithson, Jack (2025) Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts. PhD thesis, University of Nottingham. propargylation caged compounds catalysis DFT studies gold mechanism
spellingShingle propargylation
caged compounds
catalysis
DFT studies
gold
mechanism
Smithson, Jack
Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title_full Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title_fullStr Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title_full_unstemmed Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title_short Caged Compounds: A Novel Synthesis of Homocubane and its Analogues and Gold-(I) Catalysed Propargylation of Azinium Salts
title_sort caged compounds: a novel synthesis of homocubane and its analogues and gold-(i) catalysed propargylation of azinium salts
topic propargylation
caged compounds
catalysis
DFT studies
gold
mechanism
url https://eprints.nottingham.ac.uk/81034/