Selective multiboration including di- and triboration and hydroboration of alkynes and alkenes face significant challenges in organic synthesis, including achieving high regioselectivity, functional group tolerance, and catalyst stability while requiring mild conditions to maintain reactivity. These transformations have been predominantly explored by using homogeneous catalysts. In this study, we report the scalable synthesis of heterogeneous platinum single-atom catalyst (Pt-SAC) supported on ultrathin nanosheets of graphitic carbon nitride via a rapid microwave-assisted method. The Pt-SAC enables 1,2-diboration of sterically hindered alkenes and 1,2,2-triboration of alkynes with B2pin2 under mild conditions. For the diboration of styrene, the catalyst achieves 99% yield with 95% selectivity, a turnover number (TON) of 3711, and a turnover frequency (TOF) of 247 h-1. The catalyst also promotes the regioselective hydroboration of alkenes and alkynes, yielding anti-Markovnikov alkylboranes and vinylboranes, respectively. Computational calculations reveal that the enhanced reactivity on the Pt-SAC catalyst arises from adsorption-induced weakening of key bonds (C=C and B-H), thereby significantly lowering the activation energy barriers. The Pt-SAC exhibits stability and recyclability, maintaining performance over at least eight consecutive runs without detectable Pt leaching. This study highlights the potential of Pt-SAC as a robust and versatile platform for organoboron transformations under mild conditions, with relevance to applications in pharmaceutical, agrochemical, and polymer synthesis.

Center for Advanced Technologies Adam Mickiewicz University Uniwersytetu Poznańskiego 10 Poznań 61 614 Poland

Department of Industrial and Engineering Chemistry Institute of Chemical Technology Mumbai Marathwada Campus Jalna 431213 Maharashtra India

Department of Mechanical and Industrial Engineering University of Toronto 5 King's College Rd Toronto Ontario M5S 3G8 Canada

Department of Mechanical and Mechatronics Engineering Waterloo Institute for Nanotechnology Materials Interface Foundry University of Waterloo Waterloo Ontario N2L 3G1 Canada

Faculty of Chemistry Adam Mickiewicz University Uniwersytetu Poznańskiego 8 Poznań 61 614 Poland

IT4Innovations VSB Technical University of Ostrava 17 listopadu 2172 15 Ostrava Poruba 708 00 Czech Republic

Jerzy Haber Institute of Catalysis and Surface Chemistry Polish Academy of Sciences Niezapominajek 8 Krakow 30 239 Poland

Nanotechnology Centre Centre for Energy and Environmental Technologies VSB Technical University of Ostrava Ostrava Poruba 708 00 Czech Republic

Regional Centre of Advanced Technologies and Materials Czech Advanced Technology and Research Institute Palacký University Olomouc Olomouc 779 00 Czech Republic

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