Add time:09/26/2019         Source:sciencedirect.com

The reactions of [Cp∗RuCl(dippe)] and [CpRuCl(dippe)] (dippe  1,2-bis(diisopropylphosphino)ethane) with several alkynols HCCC(OH)RR′ (RR′H, Me; RMe, R′Ph) have been studied. These reactions leads to the formation of the corresponding allenylidene derivatives, although in some cases hydroxyvinylidene complexes were isolated as intermediates in such process. The X-ray crystal, structure of [CpRuCCCMePh(dippe)][BPh4] was determined. In the course of the reaction of [CpRuCl(dippe)] with HCCC(OH)Me2, there is evidence for the formation of a deep bluedimeric aklynyl-carbene (or alkenyl-allenylidene) complex [{CpRu(dippe)}2(μ-C10H11)][BPh4] resulting formally from the coupling of two allenylidene moieties followed by the loss of one proton. The reaction of [Cp∗RuCCCMePh(dippe)][BPh4] with KOBu′ leads to the ene-yne derivative [Cp∗Ru(CCC(Ph)CH2)(dippe)] as result of the deprotonation of the allenylidene ligand at the δ-position. This compound was structurally characterized by single crystal X-ray crystallography. In an attempt to obtain the primary allenylidene complex [Cp∗RuCCCH2(dippe)][BPh4] by dehydration of the hydroxyvinylidene [Cp∗RuCCHCH2OH(dippe)][BPh4] using P2O5, the previously reported carbonyl complex [Cp∗Ru(CO)(dippe)][BPh4] was obtained and its crystal structure determined. This is also accessible by aerial oxidation of the hydroxy-vinylidene derivative.

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