Concept of five-levels-four-factors central composite rotatable design was utilized for the optimization of reaction conditions of cardanol-based vinyl ester resin production, by employing response surfaces methodology, to establish a relationship between the process variables and the extent of conversion under a wide range of operating conditions which resulted in different extent of conversions. The maximum extent of conversion of cardanol-based epoxidised novolac resin (CNE) and methacrylic acid (MA) catalyzed by triphenylphosphine was found to be 95% at optimum set of conditions of molar ratio (1:0.9) between CNE and MA, catalyst concentration (1.49%), reaction temperature (89.96 degrees C) and reaction time (17,991 s). Geometrical representation of the mathematical models in three-dimensional response surface plots and isoresponse contour plots served as a good aid in understanding the behavior of reaction under different operating conditions by only limited sets of experiments. A statistical model predicted that the highest conversion yield of novolac resin would be greater than 95% at the optimized reaction conditions. The predicted values thus obtained were close to the experimental values indicating suitability of the model. (C) 2010 Elsevier B.V. All rights reserved.