An integrated pair of experiments has been developed to introduce undergraduate students to the ways in which electrochemistry can complement conventional synthetic chemistry involving redox reactions. Students first use cyclic voltammetry and linear scan voltammetry to characterize and quantify the products of the reaction between decamethylferrocene and the 4- nitrophenyldiazonium ion. In the following lab period, they synthesize the decamethylferrocenium ion as its tetrafluoroborate salt.