The reaction of α-ferrocenyl(phenyl)methanol with various azoles under the phase transfer catalysis conditions aff orded a series of ferrocenyl(alkyl)azoles in high yields. The structure of ferrocenyl(phenylmethyl)-3-trifl uoromethyl-5-(2-thienyl)pyrazole was established by X-ray diff raction. The formation of a biradical cation from the intermediately formed ferrocenyl(phenyl)carbenium ion, FcСН(Ph) + , was detected by ESR spin trap technique. Despite the demonstrated possibility of the formation of biradical cations, no products characteristic of the radical reaction pathway were found, which may serve as an indirect evidence that the reaction follows the S N 1 -mechanism.