Abstract The reaction of ribonucleoside??5′??phosphoroimidazolide with a tributylammonium orthophosphate in anhydrous dimethylformamide at room temperature provides a general method for the synthesis of nucleoside??5′??diphosphates. The novelty of the approach is to use the triethylammonium salt of 5′??monophosphate nucleoside derivative prior to the imidazolate reaction with imidazole, triphenylphosphine, and 2, 2′??dithiodipyridine. ...