An alternative method for the synthesis of biodiesel fuel from rapeseed oil that prevents formation of glycerol and produces the fuel in mass exceeding the mass of oil has been proposed. In this work the influence of reaction parameters (monoester (carboxylate ester)/oil molar ratio, catalyst concentration, temperature, reaction time) on the interesterification process was studied. The influence of catalyst structure and catalyst solvent on the interesterification process was studied, using sodium methoxide in methanol, potassium t-butoxide in t-butanol and in THF solutions. Gas chromatography methods for determination of all products and intermediates were developed. The influence of alcohol and acyl moieties of monoesters on interesterification was studied. Fuel properties of the reaction mixtures obtained with different alkyl acetates were evaluated.