Photocatalysis Minisci-type reactions involving carbon-centered radicals (CCRs) have emerged as a hot and significant topic in the field of organic synthesis chemistry. Herein, we present a nickel-vanadium nanoparticle anchored on carbon nitride catalyst (NiV-CN) and persulfate as a hydrogen atom transfer (HAT) precursor. This catalyst enables the photocatalytic Minisci-type CCR alkylation. The nickel-vanadium nanoparticles are synthesized via electrostatic attraction between [V10O28]6− anions and Ni(HCO3)2, with in situ self-assembly occurring during the hydrothermal process. In the model reaction of 4-methylquinoline with cyclohexane, the NiV-CN catalyst showed high stability, without significant loss its catalytic activity after three cycles. The CCRs was extended to cycloalkanes, adamantanes, and cyclic ethers, which react with quinoline, isoquinoline, and benzothiazole to provide the corresponding products in moderate to excellent yields. Mechanism studies indicate that nickel-vanadium nanoparticles play a crucial role in the formation process of carbon-centered radicals by activating the persulfate precursor into sulfate radicals under visible-light irradiation.

中文翻译：

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癸瓦那酸盐和 Ni（HCO3）2 自组装成锚定在氮化碳上的纳米颗粒，用于高效光催化 Minisci 型烷基化


光催化涉及碳中心自由基 （CCR） 的 Minisci 型反应已成为有机合成化学领域的热门和重要话题。在此，我们提出了一种锚定在氮化碳催化剂 （NiV-CN） 和过硫酸盐上的镍钒纳米颗粒作为氢原子转移 （HAT） 前驱体。该催化剂可实现光催化 Minisci 型 CCR 烷基化。镍钒纳米颗粒是通过 [V10O28]6− 阴离子和 Ni（HCO3）2 之间的静电吸引合成的，在水热过程中发生原位自组装。在 4-甲基喹啉与环己烷的模型反应中，NiV-CN 催化剂表现出较高的稳定性，三次循环后催化活性没有明显损失。CCR 扩展到环烷烃、金刚烷和环醚，它们与喹啉、异喹啉和苯并噻唑反应，以中等到极好的收率提供相应的产品。机理研究表明，镍钒纳米颗粒在可见光照射下将过硫酸盐前驱体活化为硫酸根自由基，在碳中心自由基的形成过程中起着至关重要的作用。