The invention relates to a preparation method of γ-substituted hexadienoic acid, which is characterized in that: (1) at 10-40°C, add a solvent, a catalyst, and a catalyst assistant to a reaction vessel, stir, and introduce oxygen, and add 1-( 2-furyl)-1-alkylcarbinol, control catalyst: catalytic promoter: the molar ratio of 1-(2-furyl)-1-alkylcarbinol is 0.0001~5:0.0001~3:100, and the reaction temperature is 0~200℃, pressure 0.1~20MPa, reaction 1~74h; solvent is a mixture of water phase and organic phase with a volume ratio of 1:0.01~3, the water phase is a phosphate acid solution, and the organic phase is a reaction inert solvent , the catalyst is a palladium compound, and the catalytic assistant is an amine or a phosphine compound; (2) cooling the reaction vessel to room temperature, adding an organic solvent for extraction, and performing vacuum distillation on the organic phase. The invention has the advantages of avoiding technical and economic disadvantages in the existing synthetic route, simplifying the technological process, reducing consumption and emission, reducing energy consumption and cost, and being suitable for industrialized production with expanded production capacity.