Diphenylphosphino functionalization of mesoporous silica using tripodal linker units

The immobilization of diphenyl phosphine onto ordered mesoporous silicas using a tripodal linker unit possessing one bromopropyl group and three anchoring silicon atoms was investigated. Solid-state 31P, 29Si, and 13C cross-polarization/magic angle spinning (CP/MAS) NMR spectroscopic studies as well as isothermal nitrogen adsorption/desorption measurements revealed that grafting the tripodal linker unit and a subsequent reaction with potassium diphenylphosphide (the “bottom-up” method) successfully realized diphenylphosphino functionalization of silica while maintaining the mesoporous structure. In contrast, directly grafting tripodal diphenylphosphino ligands pre-synthesized from the tripodal linker unit onto silica (the “top-down” method) was unsuccessful.

Graphical abstractThe immobilization of diphenyl phosphine onto ordered mesoporous silicas using a tripodal linker unit possessing one bromopropyl group and three anchoring silicon atoms was investigated. 31P, 29Si, and 13C CP/MAS NMR studies revealed that grafting the tripodal linker unit and a subsequent reaction with potassium diphenylphosphide successfully realized diphenylphosphino functionalization of silica.Figure optionsDownload full-size imageDownload as PowerPoint slideHighlights► Diphenyl phosphine was immobilized onto silica using a tripodal linker unit. ► The Br in the grafted tripodal linker unit was successfully converted into PPh2. ► Directly grafting tripodal diphenylphosphino ligands onto silica was unsuccessful.