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The electrochemical reaction of bis(acetylacetonato)palladium (Pd(acac)2) was investigated in 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)amide using a rotating ring-disk electrode. Metallic palladium was deposited on the electrode after potentiostatic cathodic reduction at −1.9 V vs. Ag|Ag(I). When the linear sweep voltammetry with maintaining the ring potential at −1.25 V was conducted, the anodic current of ring electrode was detected at −1.9 V with the cathodic disk current which is attributed to the reduction of Pd(acac)2. This result suggested that the metallic palladium may be formed by the disproportionation reaction of [Pd(acac)2]−. In addition, Pd nanoparticle was synthesized by the electrochemical reduction in 1-hexyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)amide (HMPTFSA) and 1-decyl-1-methylpyrrolidinium (DMPTFSA) in order to compare the sizes of Pd nanoparticles with that prepared in BMPTFSA. The particle size became small with increasing the alkyl chain length in the cation of ionic liquid.