A microscale laboratory is described to prepare the compounds [RuH2L(P{C6H5)3}3] (L = P(C6H5)3, H2, CO, and N2 in a pedagogical introduction to inert atmosphere inorganic syntheses. The starting material, [RuCl2{P(C6H5)3}3], is prepared routinely in 100% yield and is air-stable. The hydrogenation of this compound is accomplished using borohydride to give [RuH2L{P(C6H5)3}3] (L = P(C6H5)3 and H2). Derivatives where L = CO and N2 are prepared from [RuH2(H2){P(C6H5)3}3] by direct reaction in solution with gaseous CO and N2. 31P{1H} NMR is used to appraise the chemical purity and to determine the structures of these compounds in solution.
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