Improved syntheses Of [CP*2Mo2O5] and [CP*2W2O5]
No Thumbnail Available
Date
Journal Title
Journal ISSN
Volume Title
Publisher
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 [Cp*2M2O5] W = 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 [Cp2M2O5] 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].5H(2)O and [Cp*2W2O5] are also reported. (c) 2007 Elsevier B.V. All rights reserved.