Ribosome-Templated Azide-Alkyne Cycloadditions: Synthesis of Potent Macrolide Antibiotics by In Situ Click Chemistry.

Over half of all antibiotics target the bacterial ribosome-nature's complex, 2.5 MDa nanomachine responsible for decoding mRNA and synthesizing proteins. Macrolide antibiotics, exemplified by erythromycin, bind the 50S subunit with nM affinity and inhibit protein synthesis by blocking the passage of nascent oligopeptides. Solithromycin (1), a third-generation semisynthetic macrolide discovered by combinatorial copper-catalyzed click chemistry, was synthesized in situ by incubating either E. coli 70S ribosomes or 50S subunits with macrolide-functionalized azide 2 and 3-ethynylaniline (3) precursors. The ribosome-templated in situ click method was expanded from a binary reaction (i.e., one azide and one alkyne) to a six-component reaction (i.e., azide 2 and five alkynes) and ultimately to a 16-component reaction (i.e., azide 2 and 15 alkynes). The extent of triazole formation correlated with ribosome affinity for the anti (1,4)-regioisomers as revealed by measured Kd values. Computational analysis using the site-identification by ligand competitive saturation (SILCS) approach indicated that the relative affinity of the ligands was associated with the alteration of macrolactone+desosamine-ribosome interactions caused by the different alkynes. Protein synthesis inhibition experiments confirmed the mechanism of action. Evaluation of the minimal inhibitory concentrations (MIC) quantified the potency of the in situ click products and demonstrated the efficacy of this method in the triaging and prioritization of potent antibiotics that target the bacterial ribosome. Cell viability assays in human fibroblasts confirmed 2 and four analogues with therapeutic indices for bactericidal activity over in vitro mammalian cytotoxicity as essentially identical to solithromycin (1).

[1]  J. Heath,et al.  Protein-targeting strategy used to develop a selective inhibitor of the E17K point mutation in the PH Domain of Akt1 , 2015, Nature chemistry.

[2]  Alexander D. MacKerell,et al.  Mapping Functional Group Free Energy Patterns at Protein Occluded Sites: Nuclear Receptors and G-Protein Coupled Receptors , 2015, J. Chem. Inf. Model..

[3]  M. Disney,et al.  A toxic RNA catalyzes the in cellulo synthesis of its own inhibitor. , 2014, Angewandte Chemie.

[4]  Andrew G Myers,et al.  The evolving role of chemical synthesis in antibacterial drug discovery. , 2014, Angewandte Chemie.

[5]  S. Solomon,et al.  Antibiotic resistance threats in the United States: stepping back from the brink. , 2014, American family physician.

[6]  J. Heath,et al.  A chemical epitope-targeting strategy for protein capture agents: the serine 474 epitope of the kinase Akt2. , 2013, Angewandte Chemie.

[7]  Alexander D. MacKerell,et al.  Inclusion of Multiple Fragment Types in the Site Identification by Ligand Competitive Saturation (SILCS) Approach , 2013, J. Chem. Inf. Model..

[8]  Jocelyn T. Kim,et al.  A Cocktail of Thermally Stable, Chemically Synthesized Capture Agents for the Efficient Detection of Anti-Gp41 Antibodies from Human Sera , 2013, PloS one.

[9]  D. Scott,et al.  Fragment-based approaches in drug discovery and chemical biology. , 2012, Biochemistry.

[10]  P. Taylor,et al.  Generation of candidate ligands for nicotinic acetylcholine receptors via in situ click chemistry with a soluble acetylcholine binding protein template. , 2012, Journal of the American Chemical Society.

[11]  B. Cooperman,et al.  Real-time assay for testing components of protein synthesis , 2012, Nucleic acids research.

[12]  Roman Manetsch,et al.  Sulfo-click reaction via in situ generated thioacids and its application in kinetic target-guided synthesis. , 2012, Chemical communications.

[13]  Su Seong Lee,et al.  Iterative in situ click chemistry assembles a branched capture agent and allosteric inhibitor for Akt1. , 2011, Journal of the American Chemical Society.

[14]  Timothy R. Walsh,et al.  Tackling antibiotic resistance , 2011, Nature Reviews Microbiology.

[15]  Alexander D. MacKerell,et al.  Reproducing Crystal Binding Modes of Ligand Functional Groups Using Site-Identification by Ligand Competitive Saturation (SILCS) Simulations , 2011, J. Chem. Inf. Model..

[16]  D. Klepacki,et al.  Binding and Action of CEM-101, a New Fluoroketolide Antibiotic That Inhibits Protein Synthesis , 2010, Antimicrobial Agents and Chemotherapy.

[17]  J. Cate,et al.  Structures of the Escherichia coli ribosome with antibiotics bound near the peptidyl transferase center explain spectra of drug action , 2010, Proceedings of the National Academy of Sciences.

[18]  C. Locht,et al.  Exploring drug target flexibility using in situ click chemistry: application to a mycobacterial transcriptional regulator. , 2010, ACS chemical biology.

[19]  M. Finn,et al.  In situ click chemistry: probing the binding landscapes of biological molecules. , 2010, Chemical Society reviews.

[20]  M. Ferraro,et al.  Antimicrobial susceptibility testing: a review of general principles and contemporary practices. , 2009, Clinical infectious diseases : an official publication of the Infectious Diseases Society of America.

[21]  Alexander D. MacKerell,et al.  Computational Fragment-Based Binding Site Identification by Ligand Competitive Saturation , 2009, PLoS Comput. Biol..

[22]  Jason E Hein,et al.  Iterative in situ click chemistry creates antibody-like protein-capture agents. , 2009, Angewandte Chemie.

[23]  S. Ōmura,et al.  Chitinase inhibitors: extraction of the active framework from natural argifin and use of in situ click chemistry , 2009, The Journal of Antibiotics.

[24]  V. Fokin,et al.  Ruthenium-catalyzed azide-alkyne cycloaddition: scope and mechanism. , 2008, Journal of the American Chemical Society.

[25]  C. Gualerzi,et al.  A quantitative kinetic scheme for 70 S translation initiation complex formation. , 2007, Journal of molecular biology.

[26]  J. Fox The business of developing antibacterials , 2006, Nature Biotechnology.

[27]  K. Sharpless,et al.  In situ click chemistry: a powerful means for lead discovery , 2006, Expert opinion on drug discovery.

[28]  A. Mankin,et al.  Antibiotics and the ribosome , 2006, Molecular microbiology.

[29]  William Lindstrom,et al.  Inhibitors of HIV-1 protease by using in situ click chemistry. , 2006, Angewandte Chemie.

[30]  R. Copeland,et al.  Fluorescence Polarization Method To Characterize Macrolide-Ribosome Interactions , 2005, Antimicrobial Agents and Chemotherapy.

[31]  Zoran Radić,et al.  In situ selection of lead compounds by click chemistry: target-guided optimization of acetylcholinesterase inhibitors. , 2005, Journal of the American Chemical Society.

[32]  P. Sears,et al.  Synthesis and biological activity of new 5-O-sugar modified ketolide and 2-fluoro-ketolide antibiotics. , 2005, Bioorganic & medicinal chemistry letters.

[33]  S. Levy,et al.  Antibacterial resistance worldwide: causes, challenges and responses , 2004, Nature Medicine.

[34]  Zoran Radić,et al.  In situ click chemistry: enzyme inhibitors made to their own specifications. , 2004, Journal of the American Chemical Society.

[35]  M. Congreve,et al.  Fragment-based lead discovery , 2004, Nature Reviews Drug Discovery.

[36]  P. Dervan,et al.  DNA-templated dimerization of hairpin polyamides. , 2003, Journal of the American Chemical Society.

[37]  C. Walsh Opinion — anti-infectives: Where will new antibiotics come from? , 2003, Nature Reviews Microbiology.

[38]  Luke G Green,et al.  A stepwise huisgen cycloaddition process: copper(I)-catalyzed regioselective "ligation" of azides and terminal alkynes. , 2002, Angewandte Chemie.

[39]  P. Taylor,et al.  Click chemistry in situ: acetylcholinesterase as a reaction vessel for the selective assembly of a femtomolar inhibitor from an array of building blocks. , 2002, Angewandte Chemie.

[40]  P. Charifson,et al.  Are free energy calculations useful in practice? A comparison with rapid scoring functions for the p38 MAP kinase protein system. , 2001, Journal of medicinal chemistry.

[41]  A. Bryskier Ketolides-telithromycin, an example of a new class of antibacterial agents. , 2000, Clinical microbiology and infection : the official publication of the European Society of Clinical Microbiology and Infectious Diseases.

[42]  C. Spahn,et al.  Throwing a spanner in the works: antibiotics and the translation apparatus , 1996, Journal of Molecular Medicine.

[43]  K Schulten,et al.  VMD: visual molecular dynamics. , 1996, Journal of molecular graphics.

[44]  W. Jencks,et al.  On the attribution and additivity of binding energies. , 1981, Proceedings of the National Academy of Sciences of the United States of America.

[45]  Amethist S. Finch,et al.  Correction to A Chemically Synthesized Capture Agent Enables the Selective, Sensitive, and Robust Electrochemical Detection of Anthrax Protective Antigen. , 2018, ACS nano.

[46]  Chi-Huey Wong,et al.  In situ click chemistry: enzyme-generated inhibitors of carbonic anhydrase II. , 2004, Angewandte Chemie.

[47]  W. Jencks,et al.  Acid and base catalysis of urea synthesis: nonlinear Brønsted plots consistent with a diffusion-controlled proton-transfer mechanism and the reactions of imidazole and N-methylimidazole with cyanic acid , 1974 .