New silicon-containing disubstituted polyacetylene was prepared by the poly
merization of BTMSA having two bulky substituents (n-butyl and trimethylsil
yl) using transition metal catalysts. The polymerization proceeded in a mil
d manner and the final polymer yield was generally lower than those of sili
con-containing monosubstituted acetylenes by the similar catalyst system. T
he characterization on the polymer structure revealed that the resulting po
ly(BTMSA) have a conjugated backbone system, but the polymers have peculiar
copolymer composition of poly(BTMSA) and poly(1-hexyne) due to the spontan
eous desilylation during the polymerization. The fluoride-ion induced desil
ylation of poly(BTMSA) using n-Bu4N+F- in THF yielded a completely desilyla
ted product, pure poly(1-hexyne).