Improved syntheses of [Cp*2Mo2O5] and [Cp*2W2O5]: Structural characterization of Na[Cp∗MoO3]·5H2O and [Cp*2W2O5]
Résumé
Use of aqueous conditions and the ROOH (R = tBu or H) compounds as oxidizing agents affords a simple two-step, one-pot synthetic procedure leading to [Cp*2M2O5] (M = Mo, W) from [M(CO)6] selectively and in high yields. The hexacarbonyl compounds are converted to Na[Cp*M(CO)3] in refluxing THF, then the mixture is diluted with water (W) or aqueous NaOH (Mo) and directly treated with 6 equivalents of ROOH. Acidification of an aqueous solution of the Na[Cp*MO3] product affords spectroscopically pure [Cp*2M2O5] in high isolated yields (global yields from [M(CO)6], for R = tBu: Mo, 91%; W, 87%). The X-ray structures of Na[Cp*MoO3]∙5H2O and [Cp*2W2O5] are also reported.
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238-10.1016-j.jorganchem.2007.05.021-Accepted.pdf (612.82 Ko)
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