Analysis of silica hydride and surface hydrosilation reactions by solid-state NMR in the preparation of p-chlorobenzamide bonded silica phase.

Analytical and bioanalytical chemistry

PubMedID: 14556045

Lynch B, Müller GH, Healy LO, Glennon JD, Pursch M, Albert K. Analysis of silica hydride and surface hydrosilation reactions by solid-state NMR in the preparation of p-chlorobenzamide bonded silica phase. Anal Bioanal Chem. 2003;377(6):1014-9.
29Si and (13)C CP-MAS NMR spectroscopy was used to follow the conversion of native silica to a p-chlorobenzamide bonded silica material. The benzamide bonded phase was prepared via a hydrosilation reaction of a hydride silica intermediate with p-chloro- N-allylbenzamide. Solid-state NMR was used to show the disappearance of reactive surface hydride species (M(H)) and to identify newly formed bonded chemical species on the silica surface. DRIFT spectroscopy, elemental analysis, and specific surface-area determinations (BET) of the prepared phases are also reported.