Glycosylation reactions are most commonly encountered in nature. Synthetically, glycosylation is carried out with Lewis acid catalyst, HF, AlCl3 or mineral acids. However environmental threat associated with such catalysts has encouraged process modification and the development of solid catalyzed glycosylation reactions, which are commercially viable as well. In this contribution comparative study of glycosidic bond formation of simple D-glucose with several fatty alcohols (C-8-C-14) over variety of mixed metal oxidic spinels (CuFe2O4, ZnFe2O4, CoFe2O4 and NiFe2O4, 10% (w/w) ZnFe2O4 supported on SiO, and ZrO2) is taken up to evaluate the performance of this potential catalysts system. Effect of catalyst preparation was evaluated. This replacement of homogeneous acid catalyst by oxidic spinels shows alkyl poly beta-D-glucopyranoside as major product at comparatively low temperature range. The effects of variety of parameters were studied in a batch reactor. The mechanism of the reaction over mixed metal oxidic spinels at 363 K is put forth. (C) 2006 Elsevier B.V.. All rights reserved.