Covalent functionalization of two-dimensional molybdenum disulfide (2D MoS₂) holds great promise in developing robust organic-MoS₂ hybrid structures. Herein, for the first time, we demonstrate an approach to building up a bisfunctionalized MoS₂ hybrid structure through successively reacting activated MoS₂ with alkyl iodide and aryl diazonium salts. This approach can be utilized to modify both colloidal and substrate supported MoS₂ nanosheets. We have discovered that compared to the adducts formed through the reactions of MoS₂ with diazonium salts, those formed through the reactions of MoS₂ with alkyl iodides display higher reactivity towards further reactions with electrophiles. We are convinced that our systematic study on the formation and reactivity of covalently functionalized MoS₂ hybrids will provide some practical guidance on multi-angle tailoring of the properties of 2D MoS₂ for various potential applications.