In a process for the hydrodesulfurization of hydrocarbon feedstreams wherein said hydrocarbon feedstreams are contacted with a catalyst at a temperature and pressure and in the presence of hydrogen or a hydrogen donor solvent and under conditions sufficient to effect the hydrodesulfurization of the hydrocarbon feedstream, the improvement comprising using as the catalyst a layered material of the formula MX.sub.y wherein M is a transition metal selected from the group consisting of Group IVb, Vb, VIb, VIIb metals, X is a chalcogen selected from the group consisting of sulfur, selenium, tellurium, and mixtures thereof and y is a number ranging from about 1.5 to about 3 which material is prepared by reacting in the presence of a nonaqueous, aprotic solvent a Group IVb to VIIb metal salt, with a source of sulfide, selenide, or telluride ions, said source being selected from the group consisting of Li.sub.2 X, Na.sub.2 X, K.sub.2 X, NaHX, LiHX, KHX, (NH.sub.4)HX, (NH.sub.4).sub.2 X, (RNH.sub.3).sub.2 X, (RR'NH.sub.2).sub.2 X, (RR'R"NH).sub.2 X, wherein R, R' and R" are the same or different C.sub.1 -C.sub.20 alkyl group and C.sub.6 -C.sub.20 aryl group and X is the chalcogen selected from the group consisting of sulfur, selenium, tellurium and mixtures thereof, said reaction being conducted at a temperature of from -78.degree. to 400.degree. C. for a time sufficient for reaction to occur.