An oil⁃soluble molybdenum sulfide catalyst (MS⁃1) was prepared by a ‘one⁃pot’ synthesis method and characterized using XRD,FT⁃IR,XPS,and HR⁃TEM.The hydrodeoxygenation (HDO) performance toward methyl oleate and the hydrotreating capability for waste oils (with phosphorus,chlorine,and total metal contents of 18.14,138.80,and 173.60 µg/g,respectively) were evaluated in a high⁃pressure reactor.The results indicate that two⁃dimensional monolayer MoS2 active species were generated in situ during reaction,and the synthesized catalyst exhibited excellent overall performance.Under the conditions of a catalyst dosage of 380 µg/g,a reaction temperature of 360 °C,an initial H2 pressure of 4.0 MPa,and a reaction time of 3.0 h,the deoxygenation rates of methyl oleate and waste cooking oil reached 99.2% and 99.7%,respectively.The acid value and bromine value of the waste oil were significantly reduced from 173.60 mgKOH/g and 117.70 gBr/(100 g) to 5.28 mgKOH/g and 5.65 gBr/(100 g).The removal efficiencies of phosphorus,chlorine, and total metals were 92.17%,93.87%,and 96.92%,respectively.