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End date: 2024 × Start date: 2020 × DDC: 540 × Subject: catalysis × WGL Institute: INM ×

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    Synthesis of 3,4-Dihydro-2H-Pyrroles from Ketones, Aldehydes, and Nitro Alkanes via Hydrogenative Cyclization
    (Weinheim : Wiley-VCH, 2022) Klausfelder, Barbara; Blach, Patricia; de Jonge, Niels; Kempe, Rhett
    Syntheses of N-heterocyclic compounds that permit a flexible introduction of various substitution patterns by using inexpensive and diversely available starting materials are highly desirable. Easy to handle and reusable catalysts based on earth-abundant metals are especially attractive for these syntheses. We report here on the synthesis of 3,4-dihydro-2H-pyrroles via the hydrogenation and cyclization of nitro ketones. The latter are easily accessible from three components: a ketone, an aldehyde and a nitroalkane. Our reaction has a broad scope and 23 of the 33 products synthesized are compounds which have not yet been reported. The key to the general hydrogenation/cyclization reaction is a highly active, selective and reusable nickel catalyst, which was identified from a library of 24 earth-abundant metal catalysts.
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    Layered Nano‐Mosaic of Niobium Disulfide Heterostructures by Direct Sulfidation of Niobium Carbide MXenes for Hydrogen Evolution
    (Weinheim : Wiley-VCH, 2022) Husmann, Samantha; Torkamanzadeh, Mohammad; Liang, Kun; Majed, Ahmad; Dun, Chaochao; Urban, Jeffrey J.; Naguib, Michael; Presser, Volker
    MXene-transition metal dichalcogenide (TMD) heterostructures are synthesized through a one-step heat treatment of Nb2C and Nb4C3. These MXenes are used without delamination or any pre-treatment. Heat treatments accomplish the sacrificial transformation of these MXenes into TMD (NbS2) at 700 and 900 °C under H2S. This work investigates, for the first time, the role of starting MXene phase in the derivative morphology. It is shown that while treatment of Nb2C at 700 °C leads to the formation of pillar-like structures on the parent MXene, Nb4C3 produces nano-mosaic layered NbS2. At 900 °C, both MXene phases, of the same transition metal, fully convert into nano-mosaic layered NbS2 preserving the parent MXene's layered morphology. When tested as electrodes for hydrogen evolution reaction, Nb4C3-derived hybrids show better performance than Nb2C derivatives. The Nb4C3-derived heterostructure exhibits a low overpotential of 198 mV at 10 mA cm−2 and a Tafel slope of 122 mV dec−1, with good cycling stability in an acidic electrolyte.