Facile Synthesis of Sequence-Defined Oligo(Dimethylsiloxane-co-Diphenylsiloxane)s

1,1,3,3,5,5,7,7-Octamethyltetrasiloxane (^H MD₂ M^H ), which is reported to release Me₂ SiH₂ via a B(C₆ F₅ )₃ -catalyzed redistribution, acts as a good Me₂ SiH₂ precursor in the B(C₆ F₅ )₃ -catalyzed dehydrocarbonative condensation of alkoxysilanes. A series of oligo(dimethylsiloxane-co-diphenylsiloxane)s that are uniformly sized and sequence-defined at the atomic level are synthesized by a one-pot controlled iteration of a B(C₆ F₅ )₃ -catalyzed dehydrocarbonative condensation of alkoxysilanes with ^H MD₂ M^H or Ph₂ SiH₂ and a B(C₆ F₅ )₃ -catalyzed hydrosilylation of carbonyl compounds, followed by the subsequent B(C₆ F₅ )₃ -catalyzed dehydrogenative condensation of silanols.