In this work, we present the synthesis of multi-phase MoO3–MoSx (Mo–O–S) nanostructure as an outstanding photocatalyst through the straightforward hydrothermal method. The as-synthesized Mo–O–S nanostructure exhibited high purity and well-defined crystallite phases, featuring rods with average diameters ranging from 100–200 nm and thick flakes of 10–25 nm. The optical characterization of the as-prepared Mo–O–S nanostructure reveals four distinct emission peaks within the 520–680 nm wavelength range. The photocatalytic activity of the Mo–O–S nanostructure was evaluated through the degradation of rhodamine B (RhB), methylene blue (MB), and crystal violet (CV) dyes. The results unveil impressive degradation efficiencies, achieving 65%, 82%, and 89% after 180 min of exposure to UV irradiation for RhB, MB, and CV dyes, respectively. This pioneer investigation underscores the potential of the MoO3–MoSx nanostructure as a promising catalyst for the effective degradation of multiple dyes