Abstract A simple, high-yield synthesis is described that leads tothe sodium salt of monosulfonated triphenylphosphane (TPPMS Na) as a pure product in large quantities without complicated workup techniques. The single-crystal X-ray structure of TPPMS Na· 2.5 H 2 O is reported. The structure is built up by alternating layers of aquated sodium sulfonate units and hydrophobic triphenyl units. Thermogravimetric analyses show the loss of one ...