To treat tetramethylammonium chloride with H2SO4 in organic solvent, a precipitate is produced. A white crystallizing solid TMAHS is prepared after filtrating, washing and drying.
Then the new cage-like vinyl silsesquioxanes(VS) were synthesized by the reaction of vinyl-tetra-coordinate silicon with tetraethyl orthosilicate in the condition of tetramethylammonium hydroxide.