Syntheses of new poly (trifunctional-silyl) alkanes, which are potent coupling agents of hybrid organic–inorganic materials have been thoroughly examined. Optimization of the Benkeser reaction using chloroform, trichlorosilane and tri-n-butylamine (respective ratios 1: 4.5: 3) afforded bis (trichlorosilyl) methane isolated as bis (triethoxysilyl) methane after ethanolysis (overall yield 60%). With nine equivalents of trichlorosilane, tris (trichlorosilyl) ...