Although unconventional to most traditional synthetic chemist, electrochemistry provides a unique synthetic tool for the discovery of new and sustainable redox transformations. Considering the fundamental novel reactivity and the practical “green” features, electrochemistry thus represents a particularly attractive approach for otherwise difficult transformations in the complex settings of medicinal and material chemistry. In the field of medicinal chemistry, there remains a specific subset of transformations that are highly desirable in a drug discovery campaign. The ability to enact highly regio- and chemo selective transformations in a complex setting allows for these so called “late-stage functionalization” (LSF) strategies. In application, these LSF approaches enable medicinal chemist to introduce rapid diversification for a particular compound of interest while avoiding otherwise length de-novo syntheses. The versatility of such reactions is owed to their compatibility with a high degree of complexity as one would expect to find at the late stage of a drug compound’s development. At the same time however, this required generality makes it otherwise difficult to achieve these LSF. One particular strategy to achieve these LSF is through the use of pre-activation of otherwise unreactive C-H bonds as reactive intermediates. In this work, several methods have been developed for various LSF strategies, enabled by reactive intermediates generated through electrochemistry. The Shono oxidation, a classic electrochemical reaction, enables the oxidative activation of a C-H bonds of amine derivatives (carbamates, amides, sulfonamides) to generate iminium species, which are then trapped with an alcohol (typically the reaction solvent), to afford the corresponding N,O-acetal. Previously, access to these N,O-acetals were restricted to a limited class of simple substrates, owing to the restrictive conditions of the traditional Shono oxidation. The development of a modified Shono oxidation is reported as part of this work, laying the foundation for the LSF approaches developed in tandem. Alternative reaction conditions for the electrochemical oxidation namely the substitution of the methanol – the traditional solvent of choice for the Shono oxidation – with more oxidatively robust fluorinated alcohols, along with in-situ protecting strategies were discovered. This modified Shono oxidation system and the resulting N,O-acetals were used as highly reactive intermediates to develop LSF for a-methylation, b-fluorination, a,b-desaturation, and a,b-alkylfluorination reactions for the aforementioned amine derivatives, all of particular interest in medicinal chemistry. Additionally, preliminary reaction development for application of this modified Shono oxidation system is reported for nitramine compounds towards similar LSF of potential energetic materials. Additionally, oxidative electrochemistry was also employed for the preparation of 1,2-diamine compounds from their corresponding olefin, providing a route towards valuable synthons. In order to demonstrate the practicality of electrochemistry, this reaction was optimized at preparative scale, providing a foundation for electrochemical scale-up for real world production applications, namely by the avoidance of large amounts of stoichiometric chemical oxidants.