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使用基于氧化铁的纳米催化剂进行加氢反应合成胺。

Hydrogenation using iron oxide-based nanocatalysts for the synthesis of amines.

机构信息

Leibniz-Institut für Katalyse e.V. an der Universität Rostock, Rostock, Germany.

出版信息

Nat Protoc. 2015 Apr;10(4):548-57. doi: 10.1038/nprot.2015.025. Epub 2015 Mar 5.

Abstract

In this protocol, we describe the preparation of nanoscale iron oxide-based materials and their use in the catalysis of different hydrogenation reactions. Pyrolysis of a Fe(OAc)2-phenanthroline complex on carbon at 800 °C under argon atmosphere results in the formation of nanoscale Fe2O3 particles surrounded by nitrogen-doped graphene layers. By applying these catalysts, the hydrogenation of structurally diverse and functionalized nitroarenes to anilines proceeds with excellent selectivity. Furthermore, we have shown that one-pot reductive amination of carbonyl compounds with nitroarenes is also possible in the presence of these iron oxide catalysts. We report herein the synthesis of more than 40 amines, which are important feedstocks and key intermediates for pharmaceuticals, agrochemicals and polymers. The detailed preparation of the catalysts and the procedures for the hydrogenation processes are presented. The overall time required for the catalyst preparation and for the hydrogenation reactions are 35 h and 20-35 h, respectively.

摘要

在本方案中,我们描述了纳米氧化铁基材料的制备及其在不同加氢反应中的催化应用。在氩气氛围下,将 Fe(OAc)2-菲咯啉配合物在 800°C 下在碳上进行热解,导致纳米 Fe2O3 颗粒形成,颗粒周围是掺杂氮的石墨烯层。通过使用这些催化剂,结构多样和功能化的硝基芳烃可高效选择性地加氢为苯胺。此外,我们还表明,在这些氧化铁催化剂的存在下,羰基化合物与硝基芳烃的一锅法还原胺化也是可能的。本文报道了超过 40 种胺的合成,这些胺是制药、农化和聚合物的重要原料和关键中间体。催化剂的详细制备和加氢过程的程序都有所介绍。催化剂制备和加氢反应所需的总时间分别为 35 小时和 20-35 小时。

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