The bottom-up preparation and in-situ functionalization of MoS2 with poly(methacrylic acid) (PMAA), was accomplished. For the realization of the PMAA-MoS2 hybrid material a facile yet fast protocol based on the thermal decomposition of ammonium tetrathiomolybdate, as source for Mo and S, under microwave irradiation and in the presence of PMAA was employed. The PMAA-MoS2 was characterized by complementary spectroscopic, thermal and electron microscopy imaging techniques. Moreover, meaningful information about the dispersibility, the nature of the colloidal dispersion and the solution properties of the hybrid material were acquired by dynamic light scattering assays.