The synthesis of MCM-41-type materials functionalised with 3-mercaptopropyl(methyl)Si groups has been performed by co-condensation of the corresponding alkoxysilanes and tetramethoxysilane (TMOS), in the presence of CTAB and the amino acid leucine. The materials were oxidised to [CH3,SO3H]-MCM-41, characterised and tested as acid catalysts in the esterification of glycerol with fatty acids as lauric and oleic acids. A comparison with the performance of already reported CH3/SO3H-MCM-41 catalysts is presented.