Reaction of ferrocene with trichloroacetimidates in the presence of TMSOTf as a catalyst gave a series of novel ferrocenyl compounds, 1-7, in good yield and by a simple method using the Friedel-Crafts reaction. Only monosubstituted ferrocenyl compounds were obtained by flash chromatography at room temperature. Attempts to separate the disubstituted ferrocenyl compounds were unsuccessful, even in the presence of excess (2:1,3: 1 or 4: 1) of trichloroacetimidates. The prepared compounds have been characterized by H-1 NMR, C-13 NMR, IR, UV-vis and mass spectra as well as elemental analysis. The prepared compounds showed medium to good antimicrobial activity against Bacillus subtilis (+ve), Staphylococcus aureus (+ve), Candida albicans (yeast), Escherichia coli (-ve), Salmonella typhi (-ve), Aspergillus niger (fungi) and Fusarium solani (fungi). Copyright (c) 2005 John Wiley & Sons, Ltd.