Optimization of technological parameters for epoxidation of methallyl alcohol (MAA) by 30 wt% hydrogen peroxide was presented. The reaction was performed in a glass reactor at atmospheric pressure and in methanol (protic solvent). The titanium silicalite TS-1 catalyst was used to activate the hydrogen peroxide. The influence of the following parameters was investigated: temperature (20- 60 degrees C), MAA/ H2O2 molar ratio ( 1:1- 5: 1 mol/mol), methanol concentration (5- 90 wt %), TS-1 concentration in the reaction mixture ( 0.1- 5.0 wt %), and reaction time ( 0.5- 5 h). The optimal conditions were established by a mathematical method of design of experiments ( rotatable- uniform design). The obtained results were described using the following mathematical functions: the selectivity of transformation to 2-methylglycidol in relation to methallyl alcohol consumed, conversion of methallyl alcohol, and the selectivity of transformation to organic compounds in relation to hydrogen peroxide consumed. The courses of these functions were plotted in the system of two variables with the other parameters determining the maximum of the function.