2- ( A) and 3-dimethylchlorosilylpyridine ( B) were synthesized by reaction of the corresponding lithiopyridines with dimethyldichlorosilane at −76°C. The products were hydrolyzed in aqueous ammonia at room temperature to give the respective disiloxanes ( C and D) which are stable, colorless distillable liquids. The dimers were characterized by IR, 1H NMR and MS. The principal by-products of the syntheses were the bis-substituted derivatives. Additionally, the bis- N-oxide of D was prepared by reaction with m-chloroperoxybenzoic acid and characterized by IR, 1H NMR and MS.