Amalgamated, Oxide-Free Uranium Metal Turnings

AMALGAMATED, OXIDE-FREE URANIUM METAL TURNINGS 

In a typical procedure, approximately 30 g of uranium metal turnings are cut into small strips of approximately 0.5-1.5 in. in length using steel scissors and transferred to a 250-mL Pyrex beaker inside a well-ventilated fume hood. Concentrated nitric acid (16 M) is added to just cover the uranium turnings. The turnings are swirled with the acid approximately 1 min. 

In the glove box, 8.1 g (34.0 mmol) of freshly amalgamated uranium turnings (see Section 55.A) are placed in an oven-dried, 250-mL, one-neck Schlenk reaction vessel, along with a 1-in. Teflon-coated magnetic stirring bar, and 200 mL of distilled, degassed pyridine. The reaction vessel is removed from 

Triiodotetrakis(pyridine)uranium is an extremely air- and moisture-sensitive, purple-black solid, which may be stored for months in the absence of air and moisture. It is appreciably soluble in pyridine approximately 17 g in 30 mL pyridine at 20°C. The compound is sparingly soluble in benzene and toluene, but readily dissolves in THF with ligand substitution. Freshly prepared samples of UI3(py)4 in benzene-d6 show three broad H NMR resonances (250 MHz, 20°C) at d 17.8, 15.4, and 12.0 in a 2 1 2 ratio corresponding to the protons of coordinated pyridine.11 The IR spectrum, recorded as a Nujol mull between KBr plates, has absorptions at 1597(m), 1304(w), 1215(m), 1169(w), 1150(m), 1061(m), 1034(m), 999(m), 976(w), 756(s), 725(w), 698(s), 621(s), and 425(w)cm-1. 

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A. AMALGAMATED, OXIDE-FREE URANIUM METAL TURNINGS... 

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