The reactions of methylenediphosphanes 1a−c with hexafluoroacetone (HFA) and hexafluorothioacetone dimer (HFTA) gave the respective carbodiphosphoranes 5a, 5b, 6, 15, and 19. The carbodiphosphoranes 6 and 19, with phenyl groups at phosphorus, were able to react further with C=O or C=S functions. Compound 6 added one equivalent of HFA across one of the ylidic P=C bonds to give compound 9, a stable intermediate of the Wittig reaction. The addition of HFTA to 19 gave, unexpectedly, the isomeric compound 21. The molecular structures of 9, 15, and 21 were confirmed by X‐ray investigations.
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