The Ni-MoS2/γ-Al2O3 catalysts synthesized using thiourea solution processing. The Ni-MoS2 showed semi-amorphous crystallinity with crystallite size of 5–10 nm. The Ni K-edge XANES and EXAFS indicated the Ni substitution in MoS2 structure. A high yield of jet fuel-like hydrocarbon (>90%) from the palm kernel oil feedstock. The HDO pathway was highly selective, while the DCO2 and DCO pathways were minor.