Improved syntheses of [Cp2* Mo2 O5] and [Cp2* W2 O5]: Structural characterization of Na[Cp*MoO3] · 5H2O and [Cp2* W2 O5]
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Date
2007
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Abstract
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 [Cp2* M2 O5] (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 equiv. of ROOH. Acidification of an aqueous solution of the Na[Cp*MO3] product affords spectroscopically pure [Cp2* M2 O5] 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 [Cp2* W2 O5] are also reported. © 2007 Elsevier B.V. All rights reserved.