Kanat Zeliha, Dinçer Hatice
İstanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469, Maslak, İstanbul, Turkey.
Dalton Trans. 2014 Jun 21;43(23):8654-63. doi: 10.1039/c4dt00238e.
In order to obtain nonperipherally tetra terminal alkynyl substituted phthalocyanines (Pcs), new 3-pent-4-ynyloxy phthalonitrile (3) was prepared by the nucleophilic displacement reaction of 3-nitrophthalonitrile (1) and 4-pentyn-1-ol (2) and then cyclotetramerization was attained in the presence of zinc acetate, cobalt acetate, and/or DBU in n-pentanol without protection/deprotection. For the first time, the glycoconjugation of the nonperipherally tetra terminal alkynyl substituted zinc phthalocyanine (ZnPc) (6) can be easily achieved via the click reaction in a high yield. The electronic absorption spectrum of the glucopyranosyl substituted ZnPc (10) derivative showed a red-shifted Q band at 751 nm in dichloromethane due to the protonation of the meso nitrogens of the Pc macrocycle. Deacylation yielded ZnPc (11) bearing glucose substituents at nonperipheral positions with an improved water-solubility and non-aggregation in DMSO. The chemical structures of the new compounds were characterized by (1)H NMR, (13)C NMR, FT-IR, UV-Vis, mass spectrometry and elemental analysis. Moreover, the phthalonitrile compound was characterized using X-ray.
为了获得非周边四末端炔基取代的酞菁(Pcs),通过3-硝基邻苯二甲腈(1)与4-戊炔-1-醇(2)的亲核取代反应制备了新的3-戊-4-炔氧基邻苯二甲腈(3),然后在正戊醇中,在醋酸锌、醋酸钴和/或DBU存在下,无需保护/脱保护即可实现环四聚反应。首次通过点击反应以高产率轻松实现了非周边四末端炔基取代的锌酞菁(ZnPc)(6)的糖缀合。吡喃葡萄糖基取代的ZnPc(10)衍生物的电子吸收光谱在二氯甲烷中于751 nm处显示出红移的Q带,这是由于Pc大环的中位氮质子化所致。脱酰基反应得到在非周边位置带有葡萄糖取代基的ZnPc(11),其在DMSO中的水溶性得到改善且不聚集。通过(1)H NMR、(13)C NMR、FT-IR、UV-Vis、质谱和元素分析对新化合物的化学结构进行了表征。此外,使用X射线对邻苯二甲腈化合物进行了表征。