Department of Chemical Science and Technologies, University of Rome Tor Vergata, Via della Ricerca Scientifica 1, 00133 Rome, Italy.
Inorg Chem. 2009 Nov 2;48(21):10346-57. doi: 10.1021/ic9014866.
The reaction of 5,10,15-triarylcorrole with 4-amino-4H-1,2,4-triazole provides another example of corrole ring expansion to give the corresponding 6-azahemiporphycene, a novel porphyrin analogue. The facile oxidation of the corrole ring is a required step for the ring expansion and for this reason the reaction fails in the case of corroles bearing meso-phenyl groups carrying electron-withdrawing substituents. Steric requirements also limited the scope of the reaction, which is not successful in the case of 2,6-disubstituted meso-aryl corroles. The occurrence of an initial oxidation is further supported by formation of the 6-azahemiporphycene derivative when the reaction is carried out under the same conditions, using a 5- or a 10-isocorrole as starting material. (1)H NMR spectra and X-ray crystal characterization of 6-azahemiporphycene evidenced the presence of an intramolecular N-H...N hydrogen bond in the inner core of the macrocycle, while photophysical characterization confirmed the aromatic character of the novel macrocycle, showing an intense Soret-like band around 410 nm in the absorption spectrum. The fluorescence emission is very modest, and 6-azahemiporphycene showed higher photostability than the corresponding corrole species. Different metal complexes of 6-azahemiporphycene were prepared following synthetic protocols usually exploited for the preparation of metalloporphyrins, demonstrating good coordination properties for the macrocycle. Both the free-base and metal derivatives were characterized by cyclic voltammetry and spectroelectrochemistry in dichloromethane and benzonitrile. To further detail the behavior of this novel macrocycle, density functional theory (DFT) calculations were carried out on the basic structure of 6-azahemiporphycene with the aim of assessing aromaticity and tautomerism, as well as calculating its stability with respect to the 5-aza isomer.
5,10,15-三芳基corrole 与 4-氨基-4H-1,2,4-三唑反应提供了另一个 corrole 环扩展的例子,得到相应的 6-氮杂血卟啉,一种新型卟啉类似物。corrole 环的易氧化是环扩展的必需步骤,因此,在带有吸电子取代基的meso-苯基的 corrole 的情况下,反应失败。空间位阻的要求也限制了反应的范围,在 2,6-二取代的 meso-芳基 corrole 的情况下,反应不成功。当在相同条件下使用 5-或 10-异 corrole 作为起始原料进行反应时,形成 6-氮杂血卟啉衍生物进一步支持了初始氧化的发生。(1)H NMR 谱和 X 射线晶体表征表明,在大环的内腔中存在分子内 N-H...N 氢键,而光物理表征证实了新型大环的芳香性质,在吸收光谱中显示出大约 410nm 处的强烈 Soret 样带。荧光发射非常适中,6-氮杂血卟啉的光稳定性高于相应的 corrole 物种。根据通常用于制备金属卟啉的合成方案,制备了 6-氮杂血卟啉的不同金属配合物,证明了大环的良好配位性质。游离碱和金属衍生物均通过循环伏安法和在二氯甲烷和苯腈中的光谱电化学进行了表征。为了进一步详细研究这个新型大环的行为,使用密度泛函理论(DFT)对 6-氮杂血卟啉的基本结构进行了计算,目的是评估芳香性和互变异构体,并计算其相对于 5-氮杂异构体的稳定性。