This work explores the functionalization of an organic–inorganic MoS2 lamellar compound, prepared by a chemical liquid deposition method (CLD), that has an interlamellar distance of 5.2 nm, using clusters of gold nanoparticles. The gold nanoparticles have a mean diameter of 1.2 nm, a stability of 85 days, and a zeta potential measured to be z = 6.8 mV (solid). The nanoparticles are localized in the hydrophilic zones, defined by the presence of amine groups of the surfactant between the lamella of MoS2. SEM, TEM, EDAX and electron diffraction provide conclusive evidence of the interlamellar insertion of the gold nanoparticles in the MoS2.