Center for Drug Discovery and College of Pharmacy, University of Georgia, Athens, GA 30602, USA.
Molecules. 2013 Sep 17;18(9):11576-85. doi: 10.3390/molecules180911576.
The natural nucleoside antibiotic, bredinin, exhibits antiviral and other biological activities. While various nucleosides related to bredinin have been synthesized, its carbocyclic analog has remained unknown. Synthesis of this heretofore unknown analog of bredinin is described. The key precursor, (3aS,4R,6R,6aR)-6-((methoxy-methoxy)methyl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-amine (5), was prepared from the commercially available compound, (1R,4S)-2-azabicyclo[2.2.1] hept-5-en-3-one (4). Our initial approach used intermediate 6, derived in three transformations from 5, for the key photolytic step to produce the desired ring-opened precursor to the target compound. This photochemical transformation was unsuccessful. However, an appropriately protected and related precursor was synthesized from 5 through the following side-chain functional group transformations: elaboration of the amino group through malonyl ester formation, oximation at the central carbon, conversion of ester to amide and catalytic reduction of the oxime group. This precursor, on treatment with triethylorthoformate and catalytic acetic acid in ethanol, underwent cyclization to produce the desired 4-carbamoyl-imidazolium-5-olate ring. Deprotection of the latter product proceeded smoothly to give the carbocyclic analog of bredinin. This target molecule exhibits antiviral activity, albeit low, against a number of RNA viruses. Further biological evaluations are in progress.
天然核苷抗生素布雷迪宁具有抗病毒和其他生物活性。虽然已经合成了各种与布雷迪宁相关的核苷,但它的碳环类似物仍然未知。本文描述了这种前所未知的布雷迪宁类似物的合成。关键前体(3aS,4R,6R,6aR)-6-(甲氧基甲氧基)甲基-2,2-二甲基四氢-3aH-环戊[d][1,3]二恶烷-4-胺(5),由商业可得的化合物(1R,4S)-2-氮杂双环[2.2.1]庚-5-烯-3-酮(4)制备。我们最初的方法使用中间体 6,通过三个转化步骤从 5 中得到,用于关键的光解步骤以产生目标化合物所需的环开裂前体。这个光化学转化是不成功的。然而,从 5 经过以下侧链官能团转化合成了适当保护和相关的前体:通过丙二酰酯形成来修饰氨基,在中心碳上肟化,将酯转化为酰胺,以及催化还原肟基团。该前体在乙醇中用三乙基原甲酸酯和催化乙酸处理,通过环化反应生成所需的 4-氨甲酰基-咪唑-5-醇环。随后,该后产物的脱保护反应顺利进行,得到了布雷迪宁的碳环类似物。该靶分子表现出针对多种 RNA 病毒的抗病毒活性,尽管活性较低。进一步的生物学评价正在进行中。