mono-organothiolation of the C–H bond in ferroceneamide has been developed using aryl/alkyl disulfide substrates. The sequential ferrocene C–H organochalcogenation (chalcogen = S, Se, and Te) has also been established for the synthesis of novel hybrid unsymmetrical arylchalcogenides with the aid of a catalytic amount of Cu(OAc)2 under ambient reaction conditions. The developed protocol results in a broad functional