The MoS₂ nanocrystals coupled with anatase nanoparticles were prepared by the solvothermal method at relatively low temperatures. It was determined that the materials consisted of 15–20 nm diameter anatase nanoparticles with highly dispersed MoS₂ nanocrystals of approximately 3–7 nm in size. Visible light absorption in the MoS₂–TiO₂ samples increased with the MoS₂ content. However, their lambda edges (λ_edge) remained almost identical at approximately 390 nm, meaning that MoS₂ did not cause a red shift in the anatase bandgap energy. The hybrid MoS₂-anatase materials had higher surface area (70–124 m² g⁻¹) than commercial TiO₂ (P25) (50 m² g⁻¹). The MoS₂-anatase hybrid nanocrystals showed enhanced activity in the oxidation of methylene blue in water under UV light irradiation. A photomechanism able to elucidate the observed dye decolourisation was suggested.