Abstract Reaction of the iodides TsiSiMe 2 I and TsiSiPh 2 I,(Tsi(Me 3 Si) 3 C) with AgClO 4 in t-BuOH provides a route to the silanols TsiSiMe 2 OH and (Me 3 Si) 2-C (SiPh 2 Me)(SiMe 2 OH), respectively. TsiSiMe 2 OH gives the disiloxane TsiSiMe 2 OSiMe 3 when treated with either (a) Me 3 SiOClO 3 (prepared in situ from AgClO 4 and Me 3 SiCl) in benzene,(b) Me 3 SiI (in the presence of a little (Me 3 Si) 2-NH),(c) O, N-bis (trimethylsilyl) ...