Asymmetric Csp3-Csp3 Bond Formation via Ni-Catalyzed Regio- and Enantioselective Hydroalkylation of 1,3-Diene through Carbonyl Umpolung

29 May 2024, Version 1
This content is a preprint and has not undergone peer review at the time of posting.

Abstract

The asymmetric Csp3-Csp3 bond formation has been a grand pursuit in synthetic chemistry. The regio- and enantionselective hydroalkylation of 1,3-diene has emerged as an appealing approach for constructing chiral allylic Csp3-Csp3 bonds. However, this method is presently confined to the use of stabilized Csp3 nucleophilic substrates. Herein, we present a nickel-catalyzed asymmetric hydroalkylation of 1,3-dienes with simple unstablized alkyl carbanion enabled by hydrazones umpolung under mild reaction conditions. A range of simple alkylated chiral allylic compounds were generated in good to excellent yields, with enantiomeric ratio (er) of up to 2:98 in forming the Csp3-Csp3 bond. The protocol is applicable to heterocycles, polyenes and unsaturated hydrazones, as well as amenable for late-stage functionalizations of various complex pharmaceuticals. Density functional theory calculations elucidate the mechanism and enantioselectivity of the reaction. An enantiocontrol model is also proposed, emphasizing the crucial role of a chiral NHC ligand in facilitating this asymmetric reaction, as revealed by the two-layer two-dimensional (2D) contour maps.

Keywords

chiral Csp3-Csp3 bond
asymmetric nickel catalysis
hydroalkylation
diene
hydrazone

Supplementary materials

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Title
Asymmetric Csp3-Csp3 Bond Formation via Ni-Catalyzed Regio- and Enantioselective Hydroalkylation of 1,3-Diene through Carbonyl Umpolung
Description
The Supplementary Material provides the details of experimental procudures, the characterizations of the products, including nmr spectra, melting point, high resolution mass spectrum, HPLC spectra, etc. It also provides the details of calculation results.
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