A good-yielding two-step synthesis of RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] using conventional or microwave-assisted reflux techniques is described for use in undergraduate teaching laboratories. RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] is synthesized from RuCl[subscript 3]·xH[subscript 2]O, PPh[subscript 3], and KOH in ethanol in two steps under an inert atmosphere or using a one-pot microwave-assisted reflux to reduce the reaction time to approximately 10 min. This makes this useful compound readily available within an undergraduate laboratory session via efficient and sustainable syntheses, enabling learning outcomes associated with air-sensitive synthesis and application of group theory and spectroscopy to structure determination to be achieved.