Bis trichlorophosphoranylidene sulfamide

The syntheses of iV-trichlorophosphoranylidene derivatives (phosphazo chlorides) by the reaction of phosphorus(V) chloride with acid amides were first described by Kirsanov. When sulfamide is used, bis(trichlorophosphoranylidene)-sulfamide is obtained in nearly quantitative yield. The synthesis is effected by causing sulfamide and phosphorus (V) chloride to react in stoichiometric proportions at a controlled temperature and in the absence of a solvent. Better results are obtained, however, if the phosphorus (V) chloride is present in slight excess. If pure starting materials are used, pure bis(trichlorophosphoranylidene)sulfamide is obtained directly from the reaction mixture as a colorless viscous oil that solidifies slowly when cooled to 0°. 

Caution. Waier must be rigorously excluded during all handling or transfer operations. Filtration requires sintered- 

Bis(trichlorophosphoranylidene)sulfamide is a white, crystalline, highly hygroscopic solid that melts at 40 to 41°. It is readily soluble in benzene, diethyl ether, or carbon tetrachloride, but insoluble in n-heptane or petroleum ether 

Bis(trichlorophosphoranylidene)sulfamide is extremely reactive. Vigorous reaction occurs with water. Ckimplete replacement of the chlorine atoms is effected by treating with alcohols, phenols, amines, and organometallic compounds. 

Bis(trichlorophosphoranylidene)sulfamide is best preserved in sealed glass ampuls, although it can be stored in a vacuum desiccator over concentrated sulfuric acid or phosphorus(V) oxide. 

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