Pentafluorophenyl (fluoro) silanes (C6F5) nSiF4− n (n= 1, 2) were prepared from the corresponding ethoxysilanes by sequential chlorodeethoxylation with SOCl2 and fluoridation of chlorosilanes with SbF3. The conversion of C6F5Si (OEt) 3 and C6F5SiCl3 into C6F5SiF3 with anhydrous HF was described. Some reactions of C6F5SiF3 with electrophiles and nucleophiles were studied.