[2-(tert-Butyldimethylsilyl)phenyl]diphenyl(2,2,4,4-tetramethylpent-3-yloxy)silane (5c) is synthesized by the photolysis of 1-tert-butyl-1,1-dimethyl-2,2,2-triphenyldisilane (1c) in the presence of 2,2,4,4-tetramethyl-3-pentanone in isopentane solution at -78°C.