In this paper we report the synthesis of Vitamin K3 or Menadione by selective oxidation of 2-methyl naphthalene with H2O2 using Ti-MCM-41 synthesized by different methods. We studied the relationship between the catalytic activity and the structural characteristics and the coordination number of Ti of the catalyst. Different parameters affecting the oxidation of 2-methyl naphthalene like amount of the catalyst, hydrogen peroxide/substrate ratio, reaction temperature and the nature of the solvent are described. The experiment design-response surface methodology is used in this work to optimize the selective oxidation of 2-methyl naphthalene to vitamin K3. The application of this methodology lead us to a better understanding of the influence of the different factors (amount of catalyst, reaction temperature, H2O2 and reaction time); and their interactions, reducing the operation costs, achieving efficiency and effectiveness in this process. (C) 2004 Elsevier B.V. All rights reserved.