Silica-embedded tert-butyldimethylsilyltrifluoromethanesulfonate catalysts were synthesized by a sol-gel method in acidified CCl4, using hexadecyltrimethyl-ammonium bromide as a surfactant. The catalysts were characterized by nitrogen adsorption-desorption isotherms at 77 K; TG-DTA; H-1, C-13, and Si-29 solid state MAS/NMR; XRD; XPS; Raman spectroscopy; and FTIR after adsorption of NH3. The characterization data indicated mesoporous solids in which most of the silyl-triflate derivative keeps its integrity. The catalytic tests performed with the methyl ester of 1-cyclopentenylacetic acid in various solvents showed that the reaction selectively leads to 3-methylbenzaldehyde and is sensitive to the solvent accepting ability.