Department of Virology, Bristol-Myers Squibb Research, 5 Research Parkway, Wallingford, Connecticut 06492, USA.
Antimicrob Agents Chemother. 2011 Aug;55(8):3795-802. doi: 10.1128/AAC.00146-11. Epub 2011 May 16.
The exceptional in vitro potency of the hepatitis C virus (HCV) NS5A inhibitor BMS-790052 has translated into an in vivo effect in proof-of-concept clinical trials. Although the 50% effective concentration (EC(50)) of the initial lead, the thiazolidinone BMS-824, was ~10 nM in the replicon assay, it underwent transformation to other inhibitory species after incubation in cell culture medium. The biological profile of BMS-824, including the EC(50), the drug concentration required to reduce cell growth by 50% (CC(50)), and the resistance profile, however, remained unchanged, triggering an investigation to identify the biologically active species. High-performance liquid chromatography (HPLC) biogram fractionation of a sample of BMS-824 incubated in medium revealed that the most active fractions could readily be separated from the parental compound and retained the biological profile of BMS-824. From mass spectral and nuclear magnetic resonance data, the active species was determined to be a dimer of BMS-824 derived from an intermolecular radical-mediated reaction of the parent compound. Based upon an analysis of the structural elements of the dimer deemed necessary for anti-HCV activity, the stilbene derivative BMS-346 was synthesized. This compound exhibited excellent anti-HCV activity and showed a resistance profile similar to that of BMS-824, with changes in compound sensitivity mapped to the N terminus of NS5A. The N terminus of NS5A has been crystallized as a dimer, complementing the symmetry of BMS-346 and allowing a potential mode of inhibition of NS5A to be discussed. Identification of the stable, active pharmacophore associated with these NS5A inhibitors provided the foundation for the design of more potent inhibitors with broad genotype inhibition. This culminated in the identification of BMS-790052, a compound that preserves the symmetry discovered with BMS-346.
HCV NS5A 抑制剂 BMS-790052 的体外高效力已转化为概念验证临床试验中的体内效应。尽管最初先导化合物 BMS-824 的噻唑烷二酮在复制子测定中的 50%有效浓度 (EC(50)) 约为 10 nM,但在细胞培养基中孵育后,它会转化为其他抑制性物质。BMS-824 的生物学特征,包括 EC(50)、使细胞生长减少 50%所需的药物浓度 (CC(50)) 和耐药谱,仍然不变,这引发了对鉴定生物活性物质的研究。BMS-824 在培养基中孵育的高效液相色谱 (HPLC) 生物谱馏分显示,最活跃的馏分可以很容易地与母体化合物分离,并保留 BMS-824 的生物学特征。根据质谱和核磁共振数据,该活性物质被确定为 BMS-824 的二聚体,源自母体化合物的分子间自由基介导反应。基于对二聚体中被认为对 HCV 活性必需的结构元素的分析,合成了苯乙烯衍生物 BMS-346。该化合物表现出优异的抗 HCV 活性,并显示出与 BMS-824 相似的耐药谱,化合物敏感性的变化与 NS5A 的 N 端有关。NS5A 的 N 端已结晶为二聚体,补充了 BMS-346 的对称性,并允许讨论 NS5A 的潜在抑制模式。与这些 NS5A 抑制剂相关的稳定、活性药效团的鉴定为设计具有广泛基因型抑制作用的更有效抑制剂提供了基础。这最终导致了 BMS-790052 的鉴定,该化合物保留了与 BMS-346 发现的对称性。