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A mild one-pot reduction of phosphine(V) oxides affording phosphines(III) and their metal catalysts

Kapuśniak, Łukasz; Plessow, Philipp N.; Trzybiński, Damian; Woźniak, Krzysztof; Hofmann, Peter; Jolly, Phillip I.

Abstract:
The metal-free reduction of a range of phosphine(V) oxides employing oxalyl chloride as an activating agent and hexachlorodisilane as reducing reagent has been achieved under mild reaction conditions. The method was successfully applied to the reduction of industrial waste byproduct triphenylphosphine(V) oxide, closing the phosphorus cycle to cleanly regenerate triphenylphosphine(III). Mechanistic studies and quantum chemical calculations support the attack of the dissociated chloride anion of intermediated phosphonium salt at the silicon of the disilane as the rate-limiting step for deprotection. The exquisite purity of the resultant phosphine(III) ligands after the simple removal of volatiles under reduced pressure circumvents laborious purification prior to metalation and has permitted the facile formation of important transition metal catalysts.

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Verlagsausgabe §
DOI: 10.5445/IR/1000131419
Veröffentlicht am 16.04.2021
Originalveröffentlichung
DOI: 10.1021/acs.organomet.0c00788
Cover der Publikation
Zugehörige Institution(en) am KIT Institut für Katalyseforschung und -technologie (IKFT)
Publikationstyp Zeitschriftenaufsatz
Publikationsjahr 2021
Sprache Englisch
Identifikator ISSN: 0276-7333, 1520-6041
KITopen-ID: 1000131419
Erschienen in Organometallics
Verlag American Chemical Society (ACS)
Band 40
Seiten 693-701
Nachgewiesen in Scopus
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