An efficient method for the synthesis of ferrocenyl dithiocarbamate derivatives by means of simple condensation between dithiocarbamate and N-tosylhydrazone under green conditions is presented. This new synthetic method is metal-free, and has high yields and good functional group tolerance. Furthermore, compound 3e as a probe has shown excellent recognition of Cu²⁺ using optical and electrochemical methods. The detection limit for 3e–Cu²⁺ was 5.31 × 10⁻⁷ M.