Trichlorophenylsilane (TCP) was hydrolyzed in a toluene/water bilayer solve
nt system, and a phenylsilanetriol (PST) was produced in the aqueous layer.
To this aqueous PST solution, a phase transfer catalyst was added. The con
densation was conducted by refluxing toluene/water to obtain poly (phenylsi
lsesquioxane) (PPQS) in the toluene layer in high yield. The resultant PPQS
had a branched structure, consisting mainly of a ladder structure. In this
polycondensation, PST and the phase transfer catalyst form a salt in the a
queous layer, and this salt is transferred to the toluene layer where the c
ondensation of PST is induced.