Covalent functionalization of semiconducting MoS₂ is important in order to broaden the optoelectronic applications of this material. In the current study, we developed a one-step method for covalent edge functionalization of semiconducting MoS₂ with lipoic acid (LA). The process, which utilizes a simple sonochemical aqueous dispersion approach, generates a LA–MoS₂ conjugate that has a few layered nanoflake structure with a width of a few hundred nanometers and that display an intact crystalline basal plane. The MoS₂ conjugate has the tendency to stack and fold with random relative angles owing to the presence of LA edge linked groups.