The ability to perform air-free chemistry and catalytic reactions on an NMR tube scale are valuable skills in chemistry and not often included in undergraduate chemistry curriculum. This laboratory experiment provides students experience in synthesizing the metal complex, Ni(dcpe)(CH[subscript 3]CN)[subscript 2](BF[subscript 4])[subscript 2] (dcpe = 1,2-bis(dicyclohexylphosphino)ethane), inside an inert atmosphere glovebox, performing a catalytic alcohol oxidation reaction on a microscale, and monitoring the reaction progress by [superscript 1]H NMR spectroscopy. This activity has been employed in the Advanced Inorganic Chemistry course at Wabash College for three years. The reactions have proven to be reliable, and the students have gained valuable experience using advanced techniques common in inorganic chemistry research laboratories.