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In this work, we introduce a novel and general strategy for the environmentally friendly fabrication of mesoporous metal-organic framework (mMOF) thin films via the electrochemically assisted self-assembly (EASA) technique. Implementation of this procedure as a one-step, additive-free, and versatile protocol leads to the in situ simultaneous synthesis and deposition of mesoporous architectures of MOFs at room temperature under green conditions without the need for any base, pretreatment, or chemical modification of the underlying surface. Our procedure provides a controllable method for the synthesis of mMOF thin films (modified electrodes) consisting of hollow three-dimensional hexagonally packed crystals with two-dimensional honeycomb-like mesopores in the walls of the cavities, which grow perpendicularly onto any of the conducting surface. The resulting modified electrodes show enhanced electron transfer properties and better mass transfer performance along with the appropriate signal suitable for electrochemical sensing applications. This work can be a breakthrough and provide a new perspective for the modification and functionalization of the surface with any type of mMOF by the electrochemically driven cooperative (soft-templating) mechanism.

[reaction: see text] It is demonstrated that o-quinones, generated by the electrochemically driven oxidation of the catechols (1a-d) at physiological pH, are rapidly scavenged by 2-mercaptobenzoxazole (3) to give related catecholthioethers (4a-d) via an EC electrochemical mechanism pathway. The electrochemical syntheses of 4a-d have been successfully performed in one-pot in ambient conditions and in an undivided cell using an environmentally friendly method with high atom economy.

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Electrooxidation of 3-substituted catechols has been studied in the presence of dimedone in aqueous solution, using cyclic voltammetry and controlled-potential coulometry. The results indicate that the quinones derived from catechols participate in Michael addition reactions with dimedone to form the corresponding benzofuran derivatives (6a-c). We propose a mechanism for the electrode process. The efficient electrochemical synthesis of 6a-c has been performed at carbon rod electrodes in an undivided cell using a constant current.