Synthesis of fac-[Os(CO)3(L)Me2] (L=THF or MeCN) and some reactions with PPh3 and trityl salts
作者:Matthew J. Overett、John R. Moss
DOI:10.1016/j.ica.2004.09.052
日期:2005.3
The reaction of CiS-[Os(CO)(4)Me-2] with Me3NO in the THF or MeCN yields the complexes fac-[Os(CO)(3)(L)Me-2] (where L = THF or MeCN). Whereas the THF complex is unstable and only characterised spectroscopically, fac-[Os(CO)(3)(MeCN)Me-2] has been isolated as a white solid and fully characterized by both analytical and spectroscopic methods. These complexes fac-[Os(CO)(3)(PPh3)Me-2] are shown to be useful intermediates. Thus, reaction with PPh3 gives fac-[Os(CO)(3)(PPh3)Me-2] in good yield.Reactions of jac-[Os(CO)(3)(L)Me-2] (L = CO or MeCN) with CPh3PF6 or B(C6F5)(3) have been investigated. Whereas cis-[Os(CO)(4)Me-2] showed no reaction with either CPh3PF6 or B(C6F5)(3), the reaction of fae-[Os(CO)(3)(NleCN)Me-2] with CPh3PF6 in CH2Cl2 occurred over 16 h at room temperature to give an unstable cationic product and CPh3Me. The reaction was monitored by both IR and NMR spectroscopies. When this reaction of fac-[Os(CO)(3)(MeCN)Me-2] was carried out in the presence of a trapping ligand such as MeCN, the stable cationic product [Os(CO)(3)(MeCN)(2)Me](+) could be isolated and identified spectroscopically. (c) 2004 Elsevier B.V. All rights reserved.