Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131, Karlsruhe, Germany.
Department of Chemistry, University of Helsinki, P. O. Box 55, 00014 University of, Helsinki, Finland.
Chemistry. 2022 Jan 13;28(3):e202103511. doi: 10.1002/chem.202103511. Epub 2021 Dec 8.
This report describes the synthesis of a [2.2]paracyclophane-derived annulated 3-amino-imidazole ligand library through a Groebke-Blackburn-Bienaymé three-component reaction (GBB-3CR) approach employing formyl-cyclophanes in combination with diverse aliphatic and aromatic isocyanides and heteroaromatic amidines. The GBB-3CR process gives access to skeletally-diverse cyclophanyl imidazole ligands, namely 3-amino-imidazo[1,2-a]pyridines and imidazo[1,2-a]pyrazines. Additionally, a one-pot protocol for the GBB-3CR by an in situ generation of cyclophanyl isocyanide is demonstrated. The products were analyzed by detailed spectroscopic techniques, and the cyclophanyl imidazo[1,2-a]pyridine was confirmed unambiguously by single-crystal X-Ray crystallography. The cyclophanyl imidazole ligands can be readily transformed to showcase their useful utility in preparing N,C-palladacycles through regioselective ortho-palladation.
本报告描述了通过使用甲酰基环戊烷与各种脂肪族和芳香族异氰化物和杂芳族脒的 Groebke-Blackburn-Bienaymé 三组分反应 (GBB-3CR) 方法合成[2.2] 轮烷衍生的稠合 3-氨基-咪唑啉配体库。GBB-3CR 过程可获得骨架多样化的环戊基咪唑啉配体,即 3-氨基-咪唑并[1,2-a]吡啶和咪唑并[1,2-a]吡嗪。此外,还证明了通过原位生成环戊基异氰化物的 GBB-3CR 的一锅法。通过详细的光谱技术分析了产物,并通过单晶 X 射线晶体学明确证实了环戊基咪唑并[1,2-a]吡啶。环戊基咪唑啉配体可以很容易地转化,以展示它们在通过区域选择性邻位钯化制备 N,C-钯环方面的有用用途。