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TRIMETHYLENEMETHANE METAL COMPLEXES. PART1. SYNTHESIS OF RUTHENIUM, OSMIUM, RHODIUM, AND IRIDIUM COMPLEXES

DOI: 10.1039/DT9860001411

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1411 - 1418 (1986)

Update date:2022-08-05

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Authors:

Jones, Michael D.Jones, Michael D.

Kemmitt, Raymond D. W.Kemmitt, Raymond D. W.

Platt, Andrew W. G.Platt, Andrew W. G.

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Article abstract of DOI:10.1039/DT9860001411

1-<(Methylsulphonyloxy)methyl>-3-trimethylsilylprop-1-ene, available from 2-methylprop-2-en-1-ol, serves as a new entry into trimethylenemethane (tmm) metal complexes.Reaction with low-valent metal complexes affords the first tmm metal complexes of ruthenium, osmium, rhodium, and iridium: 4-tmm)> (M=Ru or Os), 4-tmm)>, 4-tmm)> (M=Rh or Ir), and 4-tmm)> (X=Cl, L=PPh3 or AsPh3; X=Br, L=PPh3).The desilylation of an η3-allyl intermediate rationalises the results and has been verified by the reaction of sodium fluoride with 3-CH2C(CH2SiMe3))CH2>Cl(CO)(PMe2Ph)2>BPH4 in aqueous methyl cyanide which gave the complex 4-tmm)>BPh4 in quantitative yield.N.m.r. data (1H, 13C-<1H>) are reported and variable-temperature 1H n.m.r. spin-magnetisation transfer experiments have been used to set a lower limit of ca. 90 kJ mol-1 for the activation energies for trimethylenemethane rotation.

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