Since its inception, electrochemistry has been used for synthesis of various organic compounds. Electrosynthesis features a green, scalable and single-step process in which reaction can be carried out under less harsh conditions. For example, the synthesis of benzisoxazoles by application of heterogeneous catalyzed reaction needs a combination of high pressure of hydrogen (20 bar) and use of a palladium catalyst. In the present work, electrosynthesis of 2,1-benzisoxazole and its congeners (9 examples, yield ≥ 80%) has been successfully carried out under ambient conditions and a mechanism for the reaction has been proposed through complete analysis of the reaction products. This reaction features a single-step synthesis where no catalyst is used and the initial proton donor can be recovered completely at the end of the reaction. In the second investigation, the electrochemical behavior of α,β-unsaturated ketones coupled with an ether moiety has been investigated and information obtained from this study was employed for controlled-electrodimerization of flavone to make particular hydrodimers.

In the second part of this study, controlled synthesis of copper-doped nickel tungstate, as a promising photoelectrocatalyst for the hydrogen evolution reaction has been investigated. There is an increasing need for energy generation from renewable resources and, among various options hydrogen has received the most attention. Photoelectrochemical hydrogen generation via the water-splitting reaction is a well-established topic; however, still several issues in this context remained unresolved. One of the hurdles is consolidation of the structural stability and band-gap reduction. Metal-tungsten oxides (AWO4, A = Co, Fe, Mn,…) were extensively studied for photoelectrochemical water-splitting. In this family, nickel tungstate has shown good composition stability and poor photoelectrochemical performance due to its large band-gap. Through replacing a controlled number of nickel atoms with copper ones, a new photoelectrocatalyst has been synthesized. Structural analysis revealed homogeneous copper dispersion into the nickel tungstate matrix and combination of optical and electrochemical studies also proved that the position of the energy gap is displaced in a desirable fashion.