Hybrid two-dimensional nanocomposites of transition metal semiconductors based on molybdenum disulfide, zinc oxide, and vanadium pentoxide, in which ultra-thin sheets of the inorganic component are stabilized by insertion into a bilayer of organic amphiphiles, are described. The resulting solids are commensurate species with characteristic stoichiometries, extremely high aspect ratio, and large organic-inorganic interfaces. Synthesis procedures and changes in the properties of the nanocomposites with respect to those of their components, depend on the structural nature of the pristine semiconductor. Derivatives of the laminar semiconductor MoS2 are obtained by quasi-topotactic intercalation of amphiphiles into the layered inorganic matrix, being changes in the properties mainly associated to guest-host charge transfer without altering significantly the electronic structure of the sulfide. In the case of the structurally isotropic ZnO bottom-up sol-gel synthesis procedures, it is necessary to use amphiphiles as templates, producing the two dimensional confinement with significant changes in the band gap of the semiconductor. Vanadium oxide, because of bonding asymmetry, may be easily intercalated. However due to its low laying conduction band, this leads to mixed valence species. Beyond size and dimension induced bang-gap changes, the optical properties of the products, as appreciated in their absorption and emission spectra, are in general qualitatively similar to those of pristine semiconductors.