3,4-Methylenedioxyphenol p-perfluorononenebenzonate was synthesized by esterification from p-perfluorononenebenzoyl chloride(PFNBC) and 3,4- methylenedioxy- phenol. The product was characterized by FT-IR、1H NMR、13F NMR. The effects of catalyst, reaction temperature, reaction time and the ratio of reactants on the esterification were investigated. The optimum reaction conditions of the esterification were determined as follows: n(PFNBC):n(sesamol):n(NEt3)=1:2.0:1, the reactants were agitate in DMF at -5℃ for 4h to give 3,4-methylenedioxyphenol p-perfluorononenebenzonate in the yield of 79.0 %.