THE APPLICATION OF MICROWAVE DIELECTRIC HEATING TO THE SYNTHESIS OF ARENE-METAL COMPLEXES - SYNTHESIS OF [(ETA-ARENE)(CO)(3)MN]PF6 COMPLEXES AND [(ETA-ARENE)(ETA-CYCLOPENTADIENYL)FE][PF6] COMPLEXES WITH TRIPHENYLPHOSPHINE, TERT-BUTYLBENZENES AND A STERICALLY HINDERED PHENOL AS ARENE LIGANDS
Q. Dabirmanesh et Rmg. Roberts, THE APPLICATION OF MICROWAVE DIELECTRIC HEATING TO THE SYNTHESIS OF ARENE-METAL COMPLEXES - SYNTHESIS OF [(ETA-ARENE)(CO)(3)MN]PF6 COMPLEXES AND [(ETA-ARENE)(ETA-CYCLOPENTADIENYL)FE][PF6] COMPLEXES WITH TRIPHENYLPHOSPHINE, TERT-BUTYLBENZENES AND A STERICALLY HINDERED PHENOL AS ARENE LIGANDS, Journal of organometallic chemistry, 542(1), 1997, pp. 99-103
Microwave-mediated syntheses of [(eta-arene)(CO)(3)Mn](PF6) complexes
are reported. Reaction times are reduced from several hours by convent
ional methods to a few minutes using an unmodified domestic microwave
oven. The synthesis of a bis complexed triphenylphosphine iron sandwic
h complex, [((eta-C6H5)(eta-Cp)Fe)(2) PC6H5][PF6](2) is reported from
AlCl3-catalysed ligand exchange reactions between ferrocene and M(CO)(
4)(PPh3)(2) complexes (M = Cr, Mo, W). Sterically hindered [(eta-arene
)(eta-Cp)Fe][PF6] complexes with tert-butyl substituents have been pre
pared in moderate to excellent yields using the above microwave techni
que. Attempts to synthesise the methyl cyclopentadienyl analogues resu
lted in appreciable de-alkylation. No evidence for restricted rotation
was found in the latter complexes. The direct synthesis of the 1,3,5-
trimethylphenol iron sandwich complex is reported. This is the first e
xample of a phenol complex prepared via ligand exchange reactions in i
ron sandwich chemistry. (C) 1997 Elsevier Science S.A.