Bis trifluoromethyl mercury as a Synthetic Reagent

CF3S11 bond is stable to reaction conditions that cleave the metal- halogen bond. 

The preparative reactions were conducted in sealed tubes in which l-3 g of the reagents had been placed. After the vessels had been maintained at the indicated temperatures for the designated times, the contents were removed, to be separated by fractional condensation and GLC. In addition to the (trifluoromethyl)Group 4A halides reported next, each sample contained unreacted (CFal Hg, the expected (tri-fluoromethyDmercuric halide, and the mercuric halide, identified by fluorine-NMR spectroscopy and mass spectrometry. 

In our laboratory, we find that the plasma reaction of trifiuoro-methyl radicals with mercuric iodide is an excellent source of bis(tri-fluoromethyDmercury. For those laboratories that lack access to radiofrequency (rf) equipment (a 100-W, rf source can at present be purchased for less than 1,000), synthesis of bis(trifluoromethyl)mercury by the thermal decarboxylation of (CF3C02)2Hg is also a functional, and quite convenient, source of bis(trifluoromethyl)mercury (23). 

Germanium tetraiodide (3 g) and sufficient (CFsi Hg to provide molar ratios (of mercurial to germane) of 0.55, 0.98, 1.72, and 2.00 were placed in tubes (10-mm diam.) that were then degassed, sealed, and placed in an oven held at 120°. After 120 hours, the tubes were opened, and the contents separated. The yields of the (trifluoro-methyDgermanium halides formed (16), based on Gel4, are presented in Table III. 

As these results indicate, the reaction of (CFal Hg with germanium tetraiodide provides a convenient source of the (trifluoromethyl)ger-manium iodides in good to excellent yields, and these yields can be varied, to increase the proportion of a particular (trifluoromethyl) germa- 

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