Compounds—Extra-hazardous Materials

Hewlett, in Preparative Inorganic Reactions, W. L. Jolly (ed.), Vol. 2, pp. 74-75, Interscience Publishers, a division of John Wiley Sons, Inc., New York, 1965. 

The editor is happy to acknowledge the assistance of Prof. John K. Ruff of the University of Georgia, who assisted in the preparation of this section. 

Submitted by G. W. FRASER, J. M. SHREEVE.t MAX LtJSTIG,t and CARL L. BUMGARDNER) 

Difluoroamidocarbonyl fluoride, difluoroamidosulfuryl fluoride, difluoroaminofluorosulfate, and difluoroamidosulfur penta- 

The reaction vessel is a 3-1. round Pyrex bulb equipped with a 2-mm. stopcock and a quartz tube insert (20 cm. in length and 2.5-cm. i.d.) which is sealed into the bulb by means of 45/50 S.T. joints.1,1 Fluorocarbon grease is used for lubricant. The bulb is evacuated and charged with tetrafluorohydrazine f (100-mm. pressure, 16 mmoles), which is used without purifica- 

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Difluoroa mido Compounds—Extra -hazardous Materials 303... 

Warning. Many of the nitrogen-fluorine compounds discussed in this section are very hazardous materials. Their syntheses should not be undertaken without adequate shielding equipment and a prior knowledge of techniques for the handling of explosive substances. Compounds of this type are labeled extra-hazardous or hazardous, depending upon properties of the material. 

The first method is quicker, but the filtration entailed in this reaction presents a hazard because of the danger of inhalation. If it is desired to employ volatile radioactive materials, e.g. to introduce 32P into the molecule, the second method is recommended. Further, the first method involves some danger because of the pressure developed in an enclosed reaction vessel containing ethyl chloride. It is considered essential that operations with the more volatile radioactive compounds (up to b.p. 150°/760 mm.) should be carried out in a completely enclosed system. This is possible with the second method, and the extra time of operation involves a decrease in the radioactivity of only 15 per cent compared with the first method.4... 

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