Synthesis and structure characterization of ladder-like polymethylsilsesquioxane (PMSQ) by isolation of stereoisomer

The stereo cyclic siloxane compounds having tetra hydroxyl and tetra methyl group were synthesized by hydrolysis of tetrahydrido tetramethyl cyclosiloxane consisting of four stereoisomers. Among the stereo cyclic isomers, cis-trans-cis tetrahydroxyl tetramethyl cyclosiloxane (2) was separated by recrystallization and was used as a monomer species for preparation of ladder-like polymethylsilsesquioxane (PMSQ). The isolated isomer was directly polymerized in THF with potassium carbonate (K2CO3) by systematic ring condensation. The hydrolyzed stereoisomers were characterized by 1H and 29Si NMR, and HPLC. The structure of the synthesized PMSQs were characterized by size exclusion chromatography (SEC), MALDI-TOF mass, 29Si NMR, and small angle X-ray scattering (SAXS).