Abstract: Dihydromyricetion(DMY), which was abundant and easily extracted from the leaves of Ampelopsis grossedentata, was used as the semisynthetic sources for myricetin(MYR). The structure of MYR was characterized by IR, 1H NMR and 13C NMR. Based on the results of the single factor experiments, response surface methodology(RSM) was applied to further optimize the synthesis conditions with pyridine volume fraction, and temperature, solid-liquid-ratio as the impact factors and MYR yield as the response value. The most suitable synthesis conditions of MYR were determined as follows: pyridine volume fraction 66.6%, temperature 90.4 ℃ and solid-liquid ratio 20.88(g:L). The MYR yield was 76.63%, and the relative error with the predictive value of 76.48% was 0.19%.