Assaf Khaleel I, Tehrani Foad N, Quintero Guillermo E, Hein Robert, Aliaga Margarita E, Nau Werner M
Department of Chemistry, Faculty of Science, Al-Balqa Applied University, 19117, Al-Salt, Jordan.
School of Science, Constructor University, Campus Ring 1, 28759, Bremen, Germany.
Chemistry. 2025 Feb 25;31(12):e202403964. doi: 10.1002/chem.202403964. Epub 2025 Feb 5.
The molecular confinement within rigid macrocyclic receptors can trigger catalytic activity and steer the selectivity of organic reactions. In this work, the dimerization of methylcyclopentadiene (MCPD) isomers in the presence of cucurbit[7]uril (CB7) was found to display, besides a large rate acceleration, a striking regioselectivity in aqueous solution at pH 3, different from the products predominating in the absence of the supramolecular catalyst. Among the different possible regioisomers and diastereomers, the endo-3,7-dimethyl-3a,4,7,7a-tetrahydro-1H-4,7-methanoindene adduct was selectively formed, which is otherwise found only as a minor product in the dimerization of neat MCPD or in commercial dimeric mixtures. This product originates from the reaction of the heteroternary complex of 1-MCPD and 2-MCPD within CB7, in which the methyl groups are positioned in an "anti-diaxial" arrangement and point towards the open portals of the macrocycle, resulting in a preferred packing of the reacting cyclopentadiene rings. The selectivity of the dimerization of MCPD in the absence and presence of CB7 is supported by quantum-chemical calculations.
刚性大环受体中的分子限域作用能够引发催化活性并控制有机反应的选择性。在本研究中,发现甲基环戊二烯(MCPD)异构体在葫芦[7]脲(CB7)存在下发生二聚反应时,除了反应速率大幅加快外,在pH = 3的水溶液中还表现出显著的区域选择性,这与不存在超分子催化剂时占主导的产物不同。在不同可能的区域异构体和非对映异构体中,选择性地形成了内型-3,7-二甲基-3a,4,7,7a-四氢-1H-4,7-亚甲基茚加合物,而在纯MCPD二聚反应或市售二聚体混合物中,该产物仅以微量产物形式存在。该产物源自1-MCPD和2-MCPD在CB7内形成的异三元络合物的反应,其中甲基以“反双轴”排列,指向大环的开放端口,导致反应性环戊二烯环形成优选的堆积方式。量子化学计算支持了有无CB7存在时MCPD二聚反应的选择性。