An One-pot reaction based on Algar-Flynn-Oyamada (AFO) reaction for synthesis flavonols was optimizated. Hydroxyacetophenone and the corresponding Benzaldehyde were treated as raw materials, the molar ratio of reactants, alkali, reaction solvent, reaction time, and reaction temperature were optimized through single factor test, the factors and levels, which have a greater impact on the yield of flavonols, had been screened out. On this basis, the response surface design was used for establishing a mathematical model, which could predict the flavonols’ One Pot Synthesis Process, and the mothed details were: n(corresponding benzaldehyde):n(hydroxyacetophenone):n(NaOH)=1:1.2:10.2, ethanol as solvent (0.0982 mol?L-1), reflux at 80℃ for 3h, after cooling, 35% H2O2 (0.1253 mol?L-1) and H2O (0.1253 mol?L-1) were added(the reactant aldehyde as standard), and then The reaction continued for another 3 hours at 25℃. It had been verified that the simplified synthesis process had greatly stability and extremely simply, which could effectively increase the yield of flavonols about 8.41%~23.89% and provide a method basis for the convenient synthesis of flavonols.