Abstract (C 2 F 5) 2 PCl is now accessible through a significantly improved synthesis protocol starting from the technical product (C 2 F 5) 3 PF 2.(C 2 F 5) 3 PF 2 was reduced in the first step with NaBH 4 in a solvent-free reaction at 120 C. The product, P (C 2 F 5) 3, was treated with an excess of an aqueous sodium hydroxide solution to afford the corresponding phosphinite salt Na+(C 2 F 5) 2 PO− selectively under liberation of pentafluoroethane. ...