Copper-Catalyzed Asymmetric Nitrenoid Transfer to Access Fused δ-Lactams via HFIP-Assisted Aziridination and Cascade Cyclization
Aza-steroids and terpenoid alkaloids are prominent entities of biorelevant ring-fused azacycles with significant pharmaceutical applications. Despite their importance, synthetic approaches to these complex molecules remains a great challenge due to the lack of strategic routes to the multiple contiguous chiral centers, particularly in case of thermodynamically unstable cis-ring frameworks. Herein, we report a Cu-catalyzed asymmetric cascade cyclization of arylalkenyl dioxazolones to access ring-fused δ-lactams. It is initiated to form a bicyclic N-acylaziridine intermediate to involve a concerted transition state allowing an asynchronous C–N bond formation on the open-shell singlet surface. This key reactivity is enabled by 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP), which stabilizes the reactive Cu-acylnitrenoid intermediate via inner-sphere hydrogen bonding. The resulting N-acylaziridine undergoes HFIP-promoted regio- and diastereoselective ring-opening with pendant arene or heteroarene nucleophiles to deliver condensed δ-lactam products with excellent anti-selectivity.
Authors
- Giuseppe Zanoni (ORCID: https://orcid.org/0000-0003-1530-9409)
- Young Heon Kim (ORCID: https://orcid.org/0000-0001-9944-5859)
- Suhyeon Kim (ORCID: https://orcid.org/0000-0001-7618-1854)
- Emanuele Casali (ORCID: https://orcid.org/0000-0001-7501-5213)
- Eleonora Tufano (ORCID: https://orcid.org/0009-0008-4272-6658)
- Matteo Barilli
- Dong Wook Kim (ORCID: https://orcid.org/0000-0002-5819-9783)
- Sukbok Chang (ORCID: https://orcid.org/0009-0007-9359-7502)
- Tommaso Massimini
Institutions
- Korea Advanced Institute of Science and Technology (KR)
- University of Pavia (IT)
- Institute for Basic Science (KR)
Publication Details
- Journal
- ChemRxiv
- Published
- 2025-08-22
- DOI
- https://doi.org/10.26434/chemrxiv-2025-gfjb9
- Primary Topic
- Synthesis and Catalytic Reactions
- Type
- article
- Field-Weighted Citation Impact
- 0.00
Funders
- Regione Lombardia
- Institute for Basic Science