Faculty of Pharmacy, University of Ljubljana, Aškerčeva 7, 1000 Ljubljana, Slovenia.
Int J Mol Sci. 2021 Dec 29;23(1):360. doi: 10.3390/ijms23010360.
Monocyclic ß-lactams (azetidin-2-ones) exhibit a wide range of biological activities, the most important of which are antibacterial, anticancer, and cholesterol absorption inhibitory activities. The synthesis of decorated monocyclic ß-lactams is challenging because their ring is highly constrained and consequently reactive, which is also an important determinant of their biological activity. We present the optimized synthesis of orthogonally protected 3-amino-4-substituted monocyclic ß-lactams. Among several possible synthetic approaches, Staudinger cycloaddition proved to be the most promising method for initial ring formation, yielding monocyclic ß-lactams with different substituents at the C-4 position, a phthalimido-protected 3-amino group, and a (dimethoxy)benzyl protected ring nitrogen. Challenging deprotection methods were then investigated. Oxidative cleavage with cerium ammonium nitrate and ammonia-free Birch reduction was found to be most effective for selective removal of ring nitrogen protection. Hydrazine hydrate was used for deprotection of the phthalimido group, and the procedure had to be modified by the addition of HCl in the case of aromatic substituents at the C-4 position. The presented methods and the synthesized 3-amino-4-substituted monocyclic ß-lactam derivatives are an important step toward new ß-lactams with potential pharmacological activities.
单环 β-内酰胺(氮杂环丁烷-2-酮)具有广泛的生物活性,其中最重要的是抗菌、抗癌和抑制胆固醇吸收活性。具有装饰性的单环 β-内酰胺的合成具有挑战性,因为它们的环高度受限,因此反应性强,这也是决定其生物活性的重要因素。我们提出了正交保护的 3-氨基-4-取代单环 β-内酰胺的优化合成方法。在几种可能的合成方法中,Staudinger 环加成被证明是最初环形成最有前途的方法,得到了具有不同取代基的 C-4 位、邻苯二甲酰亚氨基保护的 3-氨基和(二甲氧基)苄基保护的环氮的单环 β-内酰胺。然后研究了具有挑战性的脱保护方法。发现用硝酸铈铵和无氨 Birch 还原进行氧化裂解是选择性去除环氮保护的最有效方法。水合肼用于脱保护邻苯二甲酰亚氨基基团,但在 C-4 位具有芳基取代基的情况下,必须通过添加 HCl 来修改该程序。所提出的方法和合成的 3-氨基-4-取代单环 β-内酰胺衍生物是朝着具有潜在药理活性的新型 β-内酰胺迈出的重要一步。