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.
Authors
- Sam Butterworth (ORCID: https://orcid.org/0000-0002-6549-3753)
- Ching Ching Lam (ORCID: https://orcid.org/0000-0001-7332-5656)
- James D. F. Thompson (ORCID: https://orcid.org/0000-0002-2750-6197)
- Andrew Hackett (ORCID: https://orcid.org/0000-0001-8016-9006)
- Maneesh Kumar Reddy Singam (ORCID: https://orcid.org/0000-0002-9638-4568)
- Kendall N. Houk (ORCID: https://orcid.org/0000-0002-8387-5261)
- Christophe Aïssa (ORCID: https://orcid.org/0000-0003-0750-9435)
- Sarah Livesley
- Fernanda Duarte (ORCID: https://orcid.org/0000-0002-6062-8209)
- Craig M. Robertson (ORCID: https://orcid.org/0000-0002-4789-7607)
- James Somper
- Ana B. Garcia
Institutions
- 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)
Publication Details
- Journal
- ChemRxiv
- Published
- 2025-08-22
- DOI
- https://doi.org/10.26434/chemrxiv-2025-xv7kq
- Primary Topic
- Organic Chemistry Cycloaddition Reactions
- Type
- article
- Field-Weighted Citation Impact
- 0.00
Funders
- 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