The influence of various synthesis variables on the physico-chemical properties of mesoporous stannosilicate molecular sieves with MCM-48 structure (Sn-MCM-48) has been investigated. Sn-MCM48 has been used as a new heterogeneous catalyst in solvent-free Mukaiyama-type aldol reactions. Invariably, the beta-hydroxy ester selectivity was found to be 100% irrespective of the conversion level. The product yield was found to increase, to reach a maximum (70%), and then to decrease with the increase in tin content. (C) 2009 Elsevier B.V. All rights reserved.