Four-Component Reactions of [n.1.1]Propellanes (n = 1 or 3) Triggered by Electrophilic Activation

Exposure of [n.1.1]propellanes (n = 1 or 3) to acidic nucleophiles typically gives decomposition products due to the instability of bicyclo[n.1.1]alkyl carbocations. This instability makes the synthesis of functionalized bicyclo[n.1.1]alkanes from protic nucleophiles by electrophilic activation of [n.1.1]propellanes particularly challenging. In stark contrast, we now report a four-component reaction between [n.1.1]propellanes (n = 1 or 3), N-iodosuccinimide, nine cyclic ethers and ten classes of protic nucleophiles, that maintains the structural integrity of the bicyclo[n.1.1]alkyl motif in the products. Crucially, this reaction gives one-step access to 4-hydroxy thalidomide derivatives that enabled us to demonstrate in a whole cell assay that a n-butoxy-bicyclo[1.1.1]pentyl linker is tolerated by cereblon, a component of E3 ligase, which is an important target of proteolysis-targeting chimeras. Experimental rate law and theoretical calculations with a model nucleophile suggest that the four-component reaction relies on the attack by THF of a halogen bond complex formed between N-iodosuccinimide and the propellane, which is assisted by hydrogen bonding of the protic nucleophiles to the succinimide component.

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Journal
ChemRxiv
Published
2025-08-22
DOI
https://doi.org/10.26434/chemrxiv-2025-xv7kq
Primary Topic
Organic Chemistry Cycloaddition Reactions
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article
Field-Weighted Citation Impact
0.00

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article

Four-Component Reactions of [n.1.1]Propellanes (n = 1 or 3) Triggered by Electrophilic Activation

Sam Butterworth, Ching Ching Lam, James D. F. Thompson, Andrew Hackett et al.
ChemRxiv
Organic Chemistry Cycloaddition Reactions
article

Four-Component Reactions of [n.1.1]Propellanes (n = 1 or 3) Triggered by Electrophilic Activation

Sam Butterworth, Ching Ching Lam, James D. F. Thompson, Andrew Hackett, Maneesh Kumar Reddy Singam, Kendall N. Houk, Christophe Aïssa, Sarah Livesley, Fernanda Duarte, Craig M. Robertson, James Somper, Ana B. Garcia
article en

Abstract

Exposure of [n.1.1]propellanes (n = 1 or 3) to acidic nucleophiles typically gives decomposition products due to the instability of bicyclo[n.1.1]alkyl carbocations. This instability makes the synthesis of functionalized bicyclo[n.1.1]alkanes from protic nucleophiles by electrophilic activation of [n.1.1]propellanes particularly challenging. In stark contrast, we now report a four-component reaction between [n.1.1]propellanes (n = 1 or 3), N-iodosuccinimide, nine cyclic ethers and ten classes of protic nucleophiles, that maintains the structural integrity of the bicyclo[n.1.1]alkyl motif in the products. Crucially, this reaction gives one-step access to 4-hydroxy thalidomide derivatives that enabled us to demonstrate in a whole cell assay that a n-butoxy-bicyclo[1.1.1]pentyl linker is tolerated by cereblon, a component of E3 ligase, which is an important target of proteolysis-targeting chimeras. Experimental rate law and theoretical calculations with a model nucleophile suggest that the four-component reaction relies on the attack by THF of a halogen bond complex formed between N-iodosuccinimide and the propellane, which is assisted by hydrogen bonding of the protic nucleophiles to the succinimide component.

ChemRxiv
AstraZeneca (United Kingdom) (GB), University of Liverpool (GB), University of California, Los Angeles (US), University of Manchester (GB), University of Oxford (GB), GlaxoSmithKline (China) (CN), Smiths Detection (Canada) (CA)
National Science Foundation, Eli Lilly and Company, AstraZeneca, San Diego Supercomputer Center, University of Oxford, University of Liverpool, Croucher Foundation, Engineering and Physical Sciences Research Council, Office of Advanced Cyberinfrastructure, Division of Chemistry
Openalex Percentile: Top 84%
Organic Chemistry Cycloaddition Reactions
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