Synthesis and Catalytic Properties of Hybrid Mesoporous Materials Assembled from Polyhedral and Bridged Silsesquioxane Monomers

A family of hybrid mesoporous materials with high temperature stability was obtained by the suitable covalent combination of two types of siloxane precursors. Specifically, cubic T 8 polyhedral oligomeric (POSS) and aryl bridged silsesquioxane monomers (1,4‐bis(triethoxysilyl)benzene, BTEB) play the role of nanobuilders. An optimal molar ratio of the two precursors (5–25 mol % of total silicon content from the BTEB disilane) generated a homogenous, highly accessible, and well‐defined mesoporous material with hexagonal symmetry and narrow pore‐size distribution. Physicochemical, textural, and spectroscopic analysis corroborated the effective integration and preservation of the two different nanoprecursors, thereby confirming the framework of the mesoporous hybrid materials. A post‐synthesis amination treatment allowed the effective incorporation of amino groups onto the aryl linkers, thereby obtaining a stable and recyclable basic catalyst for use in CC bond‐formation processes.