Herein, we report an eco-friendly, electrosynthetic approach for the intramolecular oxyselenylation of allyl-naphthol/phenol derivatives.

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We report an electrochemical oxidative intramolecular cyclization reaction between 2-alkynylphenol derivatives and different diselenides species to generate a wide variety of substituted-benzo[b]furans. Driven by the galvanostatic electrolysis assembled in an undivided cell, it provided efficient transformation into oxidant-, base-, and metal-free conditions in an open system at room temperature. With satisfactory functional group compatibility, the products were obtained in good to excellent yields.

A synthetic route to obtain [p‐H2NC6H4Se]2 (1) in good yield was developed, and the crystal structure of the product was characterized for the first time. The synthesis and structure of the mercury(II) derivative [Hg(SeC6H4NH2)2] (2) was also investigated and is reported herein. The versatile coordination chemistry of [Hg(SeC6H4NH2)2] with halides of the same metal and PCy3 allows the synthesis of [Hg(X)(SeC6H4NH2)(PCy3)] (X = Cl, Br, I) (3–5). The products 1, 3–5 were isolated in crystalline form and characterized by X‐ray structure analysis.

Two new copper(II) mononuclear complexes (CSe and CS) were synthesized and characterized by the following techniques: X-ray crystallography, elemental analysis, IR, EPR and UV-Vis spectroscopies, conductimetric analysis and mass spectrometry....