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Exploration of drug design approaches with application to PIM-1 kinase and protein kinase A

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Abstract

In the context of this thesis, four distinct approaches for the design of novel inhibitors targeting PIM-1 kinase and protein kinase A (PKA) were implemented and evaluated. Design strategies were developed and selected molecules were synthesized, some following structural modification. Each approach was supported by docking and the analysis of binding modes derived from protein crystal structures or docking solutions. The objective of this work was the evaluation of different drug design strategies and the implementation of novel approaches for generating new kinase inhibitors of PIM-1 kinase and PKA. The first project involved the derivatization of an established scaffold for potential PIM-1 kinase inhibitors within a hit-to-lead optimization. To improve synthetic accessibility and facilitate structure elucidation, a quinoxaline scaffold was converted into a benzimidazole-2-carboxylic acid core. The determination of a protein crystal structure of this new fragment 20 enabled a fragment-based drug design approach, in which various growing strategies were performed via docking to explore the PIM- 1 kinase binding pocket. During this process, a pronounced instability of the free carboxylic acid was identified, preventing the successful synthesis of the planned target structures. However, the decarboxylation of several derivatives led to compounds exhibiting significant biological activity. Compound 91 emerged as the most active derivative, showing a residual PIM-1 kinase activity of 18% at an inhibitor concentration of 100 μM, thereby surpassing the biological activity of the original quinoxaline-based hit. The second project utilized a trans-stilbene hit against PIM-1 kinase as a starting point. Due to synthetic and analytical restrictions of this scaffold, it was transitioned into a structurally comparable 2-phenylbenzimidazole. This core was more synthetically accessible and bypassed the limitations of cis/trans isomerism through conformational fixation. A binding mode comparable to the stilbene hit was postulated based on docking experiments using the available protein crystal structure. On this basis, a small substance library was designed, synthesized, and biologically evaluated. However, none of the synthesized derivatives reached the potency of the starting compound, illustrating the limited transferability of structural hypotheses derived from docking studies. The third project implemented a combined strategy of ligand- and structure-based drug design. The topology of highly active, literature-known PIM-1 kinase inhibitors served as a template for scaffold hopping using FTrees. Within this framework, a workflow was developed to identify structurally related compounds from chemical spaces. A selection of these was visually evaluated regarding their synthetic accessibility and predicted binding modes in PIM-1 kinase. The six selected structures were successfully synthesized and investigated. Target compound 142 was identified as the most promising lead (45% residual activity at an inhibitor concentration of 100 μM) due to its fragment-like size. Based on 142, a SAR analysis established compound 147 as a more active bioisostere (25% residual activity). In a second design cycle, 147 was to be further optimized. The replacement of a benzene ring with a thiophene was intended to enable an interaction predicted by docking, which could not be confirmed in a protein crystal structure of PIM-1 kinase in complex with 147. Furthermore, a growing approach was aimed at establishing additional interactions. In both cases, the target structures could not be successfully synthesized due to unanticipated synthetic restrictions. The fourth project involved the implementation of a data-driven approach within a case study for the design of novel PKA inhibitors, developed in cooperation with the Volkamer group (Saarland University). The approach utilized subpocket-based docking to combine promising fragments of kinase binders into novel, highly active compounds. This led to the successful preparation of 15 compounds, synthesized in cooperation with Naemi Wagner (AK Diederich, Marburg University). Seven of these 15 compounds reduced PKA activity to below 50% at an inhibitor concentration of 100 μM, with compound 208 (6% residual activity) and compound 211 (8% residual activity) being the most active. The biological activity of 208 was further investigated, showing that it reduces PKA activity to 14% even at an inhibitor concentration of 10 μM. Consequently, several highly active PKA inhibitors were identified through this novel approach.

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Hubach, Dominik: Exploration of drug design approaches with application to PIM-1 kinase and protein kinase A. : 2026-04-20. DOI: https://doi.org/10.17192/openumr/684.

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This item has been published with the following license: In Copyright

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