Copolymerization of o-aminophenol (o-AP) and p-aminophenol (p-AP) in aqueous sulfuric acid solution was electrochemically performed using cyclic voltammetry on gold electrode. Copolymerization was carried out at different feed concentrations of homo monomers. The obtained films were characterized with cyclic voltammetry, in situ resistivity measurements, in situ UV-Vis-spectroscopy, FT-IR spectroscopy, and scanning electron microscopy (SEM). Cyclic voltammetry study shows that the onset potentials for o-AP, p-AP and o-AP + p-AP are located at the different values. The results from the electrochemical copolymerization of o-AP with p-AP demonstrate that the CVs of copolymers films growth are different from those of homopolymers, and are strongly affected by the amount of monomers. The in situ resistivity of copolymers measured from −0.20 V to 0.95 V vs. SCE decreased with increasing the [o-AP]/[p-AP] concentration ratio. In situ UV-visible and ex situ FT-IR spectra of homopolymers and copolymers results show intermediate spectroscopic behavior between homopolymers and copolymers. SEM micrographs of the samples show fundamental differences between the morphology of the homo-and copolymers.
A metal–organic framework (MOF) with sulfonic acid tags as a novel mesoporous catalyst was synthesized. The precursor of Zr-UiO-66-PDC was synthesized both via chemical and electrochemical methods. Then, zirconium-based mesoporous metal–organic framework [Zr-UiO-66-PDC-SO3H]Cl was prepared by reaction of Zr-UiO-66-PDC and SO3HCl. The structure of [Zr-UiO-66-PDC-SO3H]Cl was confirmed by FT-IR, PXRD, FE-SEM, TEM, BET, EDX, and Mapping analysis. This mesoporous [Zr-UiO-66-PDC-SO3H]Cl was successfully applied for the synthesis of dicyanomethylene pyridine derivatives via condensation of various aldehyde, 2-aminoprop-1-ene-1,1,3-tricarbonitrile and malononitrile. At the electrochemical section, a green electrochemical method has successfully employed for rapid synthesis of the zirconium-based mesoporous metal–organic framework UiO-66-PDC at room temperature and atmospheric pressure. The synthesized UiO-66-PDC has a uniform cauliflower-like structure with a 13.5 nm mean pore diameter and 1081.6 m2 g−1 surface area. The described catalyst [Zr-UiO-66-PDC-SO3H]Cl was also employed for the convergent paired electrochemical synthesis of dihydropyridine derivatives as an environmentally friendly technique under constant current at 1.0 mA cm−2 in an undivided cell. The proposed method proceeds with moderate to good yields for the model via a cooperative vinylogous anomeric based oxidation.
In this paper, the MIL-53(Al)-NH2 metal–organic frameworks (MOFs) was prepared based on the anodic electrosynthesis under green conditions. The anodic electrosynthesis as an environmentally friendly procedure was performed in the aqueous solution, room temperature, atmospheric pressure, and in the short reaction time (30 min). Also, the employed procedure was accomplished without the need for the ex-situ salt and base/probase additives as cation source and ligand activating agent at the constant current mode (10.0 mA cm−2). The electrosynthesized MOFs was functionalized with phosphorus acid tags as a novel mesoporous catalyst. This mesoporous catalyst was successfully employed for synthesis of new series (N-methyl-pyrrol)-pyrazolo[3,4-b]pyridines by one-pot condensation reaction of 3-methyl-1-phenyl-1H-pyrazol-5-amine, 3-(1-methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile and various aromatic aldehydes (mono, bis and tripodal). This catalyst proceeded the organic synthetic reaction via a cooperative vinylogous anomeric based oxidation mechanism with a marginal decreasing its catalytic activity after recycling and reusability.
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