Metal-free dehydropolymerisation of phosphine-boranes using cyclic (alkyl)(amino)carbenes as hydrogen acceptors.

Oldroyd, Nicola L; Chitnis, Saurabh S; Annibale, Vincent T; Arz, Marius I; Sparkes, Hazel A; Manners, Ian · Nat Commun · 2019

basic_science · Level V

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Abstract

The divalent carbene carbon centre in cyclic (alkyl)(amino)carbenes (CAACs) is known to exhibit transition-metal-like insertion into E-H σ-bonds (E = H, N, Si, B, P, C, O) with formation of new, strong C-E and C-H bonds. Although subsequent transformations of the products represent an attractive strategy for metal-free synthesis, few examples have been reported. Herein we describe the dehydrogenation of phosphine-boranes, RR'PH·BH<sub>3</sub>, using a CAAC, which behaves as a stoichiometric hydrogen acceptor to release monomeric phosphinoboranes, [RR'PBH<sub>2</sub>], under mild conditions. The latter species are transient intermediates that either polymerise to the corresponding polyphosphinoboranes, [RR'PBH<sub>2</sub>]<sub>n</sub> (R = Ph; R' = H, Ph or Et), or are trapped in the form of CAAC-phosphinoborane adducts, CAAC·H<sub>2</sub>BPRR' (R = R' = tBu; R = R' = Mes). In contrast to previously established methods such as transition metal-catalysed dehydrocoupling, which only yield P-monosubstituted polymers, [RHPBH<sub>2</sub>]<sub>n</sub>, the CAAC-mediated route also provides access to P-disubstituted polymers, [RR'PBH<sub>2</sub>]<sub>n</sub> (R = Ph; R' = Ph or Et).