Pentaphosphaferrocene-mediated synthesis of asymmetric organo-phosphines starting from white phosphorus.

Reichl, Stephan; Mädl, Eric; Riedlberger, Felix; Piesch, Martin; Balázs, Gábor; Seidl, Michael; Scheer, Manfred · Nat Commun · 2021

basic_science · Level V

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Abstract

The synthesis of phosphines is based on white phosphorus, which is usually converted to PCl<sub>3</sub>, to be afterwards substituted step by step in a non-atomic efficient manner. Herein, we describe an alternative efficient transition metal-mediated process to form asymmetrically substituted phosphines directly from white phosphorus (P<sub>4</sub>). Thereby, P<sub>4</sub> is converted to [Cp*Fe(η<sup>5</sup>-P<sub>5</sub>)] (1) (Cp* = η<sup>5</sup>-C<sub>5</sub>(CH<sub>3</sub>)<sub>5</sub>) in which one of the phosphorus atoms is selectively functionalized to the 1,1-diorgano-substituted complex [Cp*Fe(η<sup>4</sup>-P<sub>5</sub>R'R″)] (3). In a subsequent step, the phosphine PR'R″R‴ (R' ≠ R″ ≠ R‴ = alky, aryl) (4) is released by reacting it with a nucleophile R‴M (M = alkali metal) as racemates. The starting material 1 can be regenerated with P<sub>4</sub> and can be reused in multiple reaction cycles without isolation of the intermediates, and only the phosphine is distilled off.