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Reaction of RhCl(NBD)2 with 2.0 equiv of triphos (triphos = bis(2-diphenylphosphinoethyl)phenylphosphine; NBD = bicyclo2.2.1hepta-2,5-diene) in THF solution at room temperature affords Rh(NBD)(triphos)Cl (4a), which was isolated as Rh(NBD)(triphos)SbF6 (4b) in 67% yield. Treatment of 4b with aqueous formaldehyde in THF solution at 80 °C forms Rh(CO)(triphos)SbF6 (2a), which reversibly binds a second equivalent of CO(g) to give Rh(CO)2(triphos)SbF6 (2b). The complex Rh(CO)(triphos)SbF6 has been found to be an effective aldehyde decarbonylation catalyst for primary and aryl aldehydes at temperatures as low as that of refluxing dioxane, with little or no undesirable side products resulting from β elimination or radical rearrangement.
Beck et al. (Wed,) studied this question.