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A general protocol for the selective hydrogenation and deuteration of a variety of alkenes is presented. Key to success for these reactions is the use of a specific nickel‐graphitic shell‐based core–shell‐structured catalyst, which is conveniently prepared by impregnation and subsequent calcination of nickel nitrate on carbon at 450 °C under argon. Applying this nanostructured catalyst, both terminal and internal alkenes, which are of industrial and commercial importance, were selectively hydrogenated and deuterated at ambient conditions (room temperature, using 1 bar hydrogen or 1 bar deuterium), giving access to the corresponding alkanes and deuterium‐labeled alkanes in good to excellent yields. The synthetic utility and practicability of this Ni‐based hydrogenation protocol is demonstrated by gram‐scale reactions as well as efficient catalyst recycling experiments.

Ambient Hydrogenation and Deuteration of Alkenes Using a Nanostructured Ni‐Core–Shell Catalyst