Abstract Transition metal-substituted carboxylic acids, MRCOOH (R= CH 2, CH 2 CH 2), are prepared by the reactions of metal anions with trimethylsilyl halocarboxylates, XRCOOSiMe 3, followed by treatment with silica gel. The carboxylic acid moiety is readily transformed into various acyl derivatives MRCONu such as esters and amides via an acyl chloride intermediate, MRCOCl.