Low temperature synthesis of ionic phosphates in dimethyl sulfoxide

Abstract

A new synthesis route for phosphates in an organic solvent at low temperatures is presented. The synthesis was done by dispersing a nitrate salt and phosphorus pentoxide in dimethyl sulfoxide. The synthesis can be performed under water-free conditions and yielded several organic and inorganic phosphates. Crystal structure solution of bistetramethylammonium hydrogencyclotriphosphate, [N(CH₃)₄]₂HP₃O₉, was achieved by combining information gained from powder X-ray diffraction, liquid NMR and solid state (2D) NMR. The molecular structure of rubidium cyclotetraphosphate, Rb₄P₄O₁₂, was determined using liquid state NMR and solid state (2D) NMR spectroscopy.