Abstract

Nano-α-Fe₂O₃ prepared using acid pickling waste as precursor was found to be an effective catalyst for benzylation aniline with benzyl chloride. However, the formation of a green solution was observed during the solvent-free benzylation. A yellow-green single crystal as a byproduct was recovered from the green reaction mixture and characterized by X-ray single crystal diffraction, ¹H NMR, FT-IR and elemental analysis. The results showed that this single crystal was a composite structural complex constructed by [(C₆H₆–CH₂)₂NH–C₆H₆]FeCl₄ and [(C₆H₆–CH₂)₂NH–C₆H₆]Cl in equimolar ratio. The formation of the complex led to the deactivation and non-reusability of α-Fe₂O₃ catalyst for catalyzing solvent-free N-benzylation of aniline with benzyl chloride. The forming mechanism of the crystal was also discussed.

中文翻译：

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苯甲酰氯在无溶剂苯胺的N-苄基化反应中氧化铁催化剂失活的研究

摘要

纳米的α-Fe ₂ ö ₃使用酸洗废弃物作为前体被认为是对与苄基氯苄化苯胺的有效催化剂制备。但是，在无溶剂的苄基化过程中观察到绿色溶液的形成。从绿色反应混合物中回收作为副产物的黄绿色单晶，并通过X射线单晶衍射，¹ H NMR，FT-IR和元素分析对其进行表征。结果表明，该单晶是由[（C ₆ H ₆ -CH ₂）₂ NH-C ₆ H ₆ ] FeCl ₄和[（C ₆ H₆ -CH ₂）₂ NH-C ₆ H ₆ ] Cl等摩尔比。复杂导致失活和的α-Fe的不可再利用的形成₂ ö ₃用于催化无溶剂苯胺与苄基氯的N-苄基化催化剂。还讨论了晶体的形成机理。