Nickel-molybdenum sulfide catalysts have been synthesized in situ in a hydrocarbon medium by the decomposition of the [(n-Bu)(4)N](2)Ni(MoS4)(2) precursor complex supported on an ordered mesoporous phenol-formaldehyde polymer in the presence of a sulfiding agent (dimethyl disulfide). The catalytic properties of the samples have been studied in a batch reactor at 380A degrees C and a hydrogen pressure of 5.0 MPa using the example of naphthalene, 1-methylnaphthalene, and 2-methylnaphthalene. The tests have shown that the conversion of biaromatic substrates is close to quantitative and the use of dimethyl disulfide as a sulfiding agent leads to an increase in the amount of complete hydrogenation products, as evidenced by the high content of the active phase in this case.