Showing posts with label tuberculosis. Show all posts
Showing posts with label tuberculosis. Show all posts

18 December 2023

Review of 2023 reviews

The annual Practical Fragments look-back on the preceding year may not be the most highly anticipated year-end tradition, but I hope you find something of interest in this twelfth edition.
 
I was fortunate to attend several conferences and wrote about CHI’s Discovery on Target in Boston and Drug Discovery Chemistry in San Diego. As for reviews, Louise Walsh and collaborators at Astex, Vrije Universiteit Amsterdam, Novartis, and Frontier Medicines (me!) published our annual analysis of fragment-to-lead success stories in J. Med. Chem., this one covering the year 2021. Some twenty other reviews of interest to this readership were also published. I’ll cover them thematically below.
 
Methods
Crystallography is the most popular fragment-finding technique, and in Expert Opin. Drug Disc. Wladek Minor and collaborators at University of Virginia and Jagiellonian University examine “the current role and evolution of X-ray crystallography in drug discovery and development.” At the start of 2023 the Protein Data Bank (PDB) contained more than 200,000 structures, which sounds impressive until you learn that the AlphaFold database contains more than 200 million predicted protein structures. But this is not experimentalist vs machine: the researchers note how machine learning approaches can be used to more rapidly refine and improve experimental data with resources such as CheckMyBlob and PDB-REDO.
 
For those wishing to dig deeper, two papers in Methods Enzymol. go into experimental detail. In the first, Natalie Tatum and colleagues at Newcastle University describe “crystallographic fragment screening in academic drug discovery.” May Sharpe and collaborators at the Swiss Light Source and University of Hohenheim describe their fast fragment-screening pipeline in a comprehensive (49 page) guide. The focus is on reproducibility, and there is plenty of practical advice. For example, “the authors have even been successful in flying with crystal plates,” though getting these through airport security may be easier in some countries than others.
 
Protein-detected NMR was the first truly practical fragment-based approach, and another paper in Methods Enzymol. by Brian Volkman, Brian Smith, and colleagues at Medical College of Wisconsin describes “fragment-screening by protein-detected NMR.” This distills eight years of effort building their internal protein-detected NMR fragment screening platform that has been applied to 16 proteins thus far. The chapter is particularly detailed on protein and library preparation and screening.
 
Compared with crystallography and NMR, virtual screening can be dramatically faster; we’ve highlighted multibillion-compound screens. In WIREs Comput. Mol. Sci., Artem Cherkasov, Francesco Gentile, and colleagues at University of British Columbia and University of Ottawa discuss (open access) how computational methods are “keeping pace with the explosive growth of chemical libraries.” They cover brute force methods, fragment-based virtual screening, and machine-learning based methods, all while avoiding hype, and conclude that it will take time for these methods to “have a real impact on practical drug discovery.”
 
Finally, Marianne Fillet and collaborators at University of Liege and University of Namur provide a general review in Trends Anal. Chem. covering multiple methods to detect non-covalent fragments. These include established techniques such as biochemical assays, ligand-observed NMR, crystallography, thermal shifts, and SPR, as well as less common ones such as WAC, microscale thermophoresis, ACE, and DEL. The paper includes several nice tables and even a decision tree to help choose among the various approaches.
 
Covalent fragments
Many techniques to detect noncovalent interactions also apply to reversible covalent inhibitors, the subject of a review in Med. Chem. Res. by Faridoon and collaborators at Genhouse Bio and Olema Oncology. The researchers focus on various warheads including cyanoacrylamides, nitriles, ketones and aldehydes, boronic acids, and others, and provide multiple examples for each.
 
In contrast, an open-access review in Pharmaceuticals by Monique Multeder and collaborators at Leiden University Medical Center discusses methods to detect both reversible as well as irreversible covalent protein-drug adducts. Crystallography is the most informative, but the researchers also delve into various mass-spectrometry techniques including top-down (with intact proteins) and bottom-up (after digestion of modified proteins). Also covered are activity-based protein profiling (ABPP) methods, NMR, and fluorescence-based approaches. The nearly 300 references make a useful compendium.
 
One of the most exciting recent developments is “proteome-wide fragment-based ligand and target discovery,” the subject of an open-access review in Isr. J. Chem. by Ines Forrest and Christopher Parker, both at Scripps. This concise, highly readable account covers a lot of ground, from ABPP to fully functionalized fragments (FFFs) to phenotypic screening.
 
If you’re doing covalent FBLD you’ll need a library of covalent fragments, and if you’re building one, I’d recommend a review in Prog. Med. Chem. by David Mann and colleagues at Imperial College London. The paper nicely summarizes design principles such as choice of warhead and the fact that reactivity can vary considerably even among compounds with the same warhead. Synthetic methods and screening approaches are also well covered, along with methods to distinguish specific binding from nonspecific reactivity.
 
Most covalent fragments target cysteine residues, but there at least nine other potentially reactive amino acids, and these are the subject of an open-access review by György Keserű and colleagues at Budapest University of Technology and Economics in Trends Pharm. Sci. Lysine, serine, threonine, tyrosine, and histidine are the most common targets, though some of the warheads are so reactive that specificity will be challenging, let alone reasonable pharmacokinetic properties. This is especially true for aspartic and glutamic acids, methionine, and tryptophan.
 
Finally, another article in Trends Pharm. Sci. by Carlo Ballatore and colleagues at University of California San Diego describes using covalent strategies to develop stabilizers and inhibitors of protein-protein interactions (PPIs). Site-directed fragment tethering with disulfide and imine chemistry is a focus, particularly in the context of 14-3-3 proteins. Proximity-enabled covalent strategies, in which warheads are grafted onto non-covalent molecules, are also covered. There is also a short section on covalent PROTACs – more on that topic below.
 
Targets
Keeping with the theme of protein-protein interactions, Ge-Fei Hao, Guang-Fu Yang, and collaborators at Central China Normal University and Guizhou University discuss fragment-based approaches against “undruggable” PPIs in Trends Biochem. Sci. After describing why protein-protein interactions can be difficult, the paper presents several successful case studies, including venetoclax, sotorasib, and targeting 14-3-3 proteins.
 
Targeted protein degradation continues to be a major focus for drug discovery, and this is commonly achieved by hijacking E3 ligases to cause them to ubiquitinate a target of interest. Iacovos Michaelides and Gavin Collie (AstraZeneca) describe how FBLD has been used to find ligands against E3s in an open-access J. Med. Chem. paper. There are more than 600 E3s, and because their biology relies on protein-protein interactions they are often tough targets. Fragment hits can be weak and difficult to advance, though the researchers do describe several success stories including against KEAP1 and XIAP/cIAP. Covalent fragments have the potential to permanently reprogram E3 ligases, and these are covered well too.
 
Another difficult type of target is RNA, the topic of two reviews. In an open-access Curr. Opin. Struct. Biol. paper Kevin Weeks and colleagues at University of North Carolina Chapel Hill provide a concise and beautifully illustrated overview of the field. They note that “RNA-targeted FBLD is in its infancy,” but given that the first report dates to 2002 it is a long childhood, and the paper does a good job of describing the challenges.
 
A more extensive treatment of “fragment-based approaches to identify RNA binders” is provided by Matthew Disney and colleagues at UF Scripps in J. Med. Chem. The paper describes many case studies, some of which we’ve covered, and also contains a handy table comparing the pros and cons of a dozen different methods for finding RNA-binding fragments.
 
Tuberculosis kills more than 1.5 million people each year, and fragment-based approaches have been applied against multiple targets within the pathogen, as reviewed by Baptiste Villemagne and colleagues at University Lille in Eur. J. Med. Chem. We’ve covered many of these studies on Practical Fragments, but as the paper notes none have advanced to the clinic. This is attributed in part to cell permeability, and the researchers suggest turning to phenotypic screens (see below).
 
Other
Fragment linking can be difficult but highly effective, especially for difficult targets. An overview of published linkers is provided by Isabelle Krimm and collaborators at Université Claude Bernard Lyon and Université Montpellier in Expert Opin. Drug Disc. The paper includes a table summarizing 40 fragment linking stories, noting that most linkers are short and flexible. Another table summarizes 19 examples of target-guided synthesis, including dynamic combinatorial chemistry. As the paper notes, all of these are small model studies based on known compounds. In silico approaches, the last topic covered, will probably prove more practical.
 
And on the subject of practical, Dean Brown (Jnana Therapeutics) provides an “analysis of successful hit-to-clinical candidate pairs” in J. Med. Chem. This is an update to his 2018 article and captures 156 clinical candidates reported in the journal between 2018 and 2021. Of these, 14 had fragments in their lineage. Most of these drugs appear in our list of fragment-derived clinical candidates (though berotralstat does not – I’ll need to look closer). The paper contains lots of interesting analyses. For example, of the 138 oral drugs, 39 had a molecular weight > 500 Da, 24 had Clog > 5, and 17 had more than 10 hydrogen bond acceptors (HBA). On the other hand, none had more than 5 HBD, emphasizing that you should be parsimonious with hydrogen bond donors.
 
Finally, veteran drug hunter Nicholas Meanwell provides “reflections on a 40-year career in drug design and discovery” (open access) in Med. Chem. Rev. Those of you who saw his talk earlier this year at the CHI DDC meeting will know what to expect, and those of you who didn’t will be in for a treat. A personal and entertaining romp through pharma starting in the early 1980s, the paper is full of surprises, such as the pursuit of minor impurities in a phenotypic screen that ultimately led to the hepatitis C drug daclatasvir. Nicholas notes that “you discover what you screen for, so screen design is of paramount importance.”
 
The paper also reveals a passion for medicinal chemistry: “In a search for inspiration for design concepts, I sat down one Saturday afternoon in early October of 1987 and perused every molecule in the United States Adopted Names (USAN) dictionary.” And, as he notes near the end, “Decision making in drug discovery and development is a delicate balancing act, inherently flawed based on absence of predictive accuracy, and knowing when to conclude a discovery program with grace is also an important trait.” That said, he provides examples of successful programs that were almost killed multiple times – and others that were killed at Bristol Myers Squibb but subsequently succeeded elsewhere. While this is frustrating on one level, Nicholas takes satisfaction in the fact that “the science that we conducted and the molecules and pharmacophores that we defined have been of benefit to mankind.”
 
There are still a couple weeks left in the year, but that’s it for Practical Fragments for 2023. Thanks for reading, and special thanks for commenting. And if you live in one of the 70+ countries with elections in 2024, please vote.

28 June 2021

Twenty seven hits against four tuberculosis targets

1.2 million deaths. If you did not read the title of this post carefully you may assume this statistic refers to COVID-19. In fact, it is the number of people who died of tuberculosis in 2019. Worse, drug resistant forms of Mycobacterium tuberculosis, the organism that causes TB, are spreading far faster than new treatments are being developed. Initial efforts at addressing this problem are reported (open access) in Comp. Struct. Biotech. J. by Sangeeta Tiwari (University of Texas El Paso), Vitor Mendes (University of Cambridge) and a multinational team of collaborators.
 
M. tuberculosis is capable of making all 20 amino acids. The bug can also scavenge arginine from its host, but only inefficiently: knocking out the biosynthetic pathway abolishes virulence. Thus, targeting this pathway might lead to new drugs.
 
In total eight enzymes are needed to synthesize L-arginine from L-glutamate, and the researchers targeted four of them. The proteins were screened against a library of 960 fragments (each at 5 mM) using differential scanning fluorimetry (DSF). Depending on the specific target some of the hits were validated by SPR or ligand-based NMR before being taken into crystallography, which yielded structures of all the enzymes. In total 13 fragments were found to bind to ArgB, 4 bound to ArgC, 2 bound to ArgD, and 8 bound to ArgF. All the coordinates have been deposited in the protein data bank, though they don’t seem to have been released as of June 28.
 
The paper details the binding interactions for all the hits. Most of them are quite weak, though two hits against ArgB have low micromolar dissociation constants as assessed by ITC. Tantalizingly, these inhibit the growth of M. tuberculosis, and one of them seems to be on-target (adding arginine to the media rescues the inhibition). All the ArgB fragments bind not at the active site but rather at an interface between protein subunits. Unfortunately this site is quite hydrophobic, as are the fragments, suggesting an uphill battle in optimization.
 
A good antibiotic should not hit human proteins, and neither ArgB nor ArgC have human orthologs. ArgF does, but the region where the fragments bind is quite different. ArgD, with only two crystallographically-confirmed hits and 36% identity to the human enzyme, is probably the least attractive.
 
A year before the COVID-19 Moonshot launched we highlighted the Open Source Antibiotics initiative. I don’t think that team was involved with this research, but they would seem to be a natural fit. If you have spare bandwidth and are looking to do some fragment to lead optimization, this paper provides more than two dozen starting points.

26 December 2016

Review of 2016 reviews

This year is finally coming to an end, and as we've done for the past four years, Practical Fragments will highlight some of the reviews that we didn't cover previously.

In terms of what we did cover, there were several excellent events, including the eleventh annual CHI FBDD Conference in San Diego, an inaugural meeting in Houston, and of course the first-ever major fragment event in Boston, FBLD 2016.

The twentieth anniversary of SAR by NMR was also commemorated by the eighth book devoted to FBLD, as well as a massive two volume work on lead generation. We also covered a special issue of Molecules and reviews on clinical candidates and library design.

Another review on library design was published recently in Drug Disc. Today by Ian Gilbert, Paul Wyatt, and colleagues at the University of Dundee. The researchers have built a set of 356 diverse compounds consisting of “capped” scaffolds, such that any hits could be rapidly expanded. Undergraduates did much of the actual library assembly, learning skills such as parallel chemistry and how to work with polar compounds. There is lots of nice detail in this paper, including on library storage conditions.

Targets
Practical Fragments often highlights successful fragment to lead programs, and these were the focus of a Perspective in J. Med. Chem. by Christopher Johnson (Astex) and collaborators: all 27 cases published in 2015 in which the affinity of a fragment was improved at least 100-fold to a 2 µM or better lead. Many of these were covered in Practical Fragments, including BTK, DDR1/2, ERK2, MELK, Mtb TMK, PKCθ, RET, FactorXIa, MMP-13, BCATm, PDE10A, soluble epoxide hydrolase, tankyrase, ATAD2, MCL-1, RAD51, XIAP/cIAP, and mGluR5. The paper also draws general conclusions about target types, molecular weights, cLogP values, and LE.

Targeting tuberculosis (TB) is the subject of two reviews from University of Cambridge researchers, one in Drug Discov. Today by Vitor Mendes and Tom Blundell and one in Parasitology by Anthony Coyne, Chris Abell, and colleagues. Fragment-based approaches have been more or less successful against several TB proteins, including pantothenate synthetase, CYP121, BioA, EthR, and thymidylate kinase, while other targets – such as shikimate kinase and CYP144 – have proven more difficult.

July was bromodomain month at Practical Fragments, and this target class is the subject of a review in Drug Discov. Today: Technol. by Dimitrios Spiliotopoulos and Amedeo Caflisch at the University of Zurich. The focus is on computational fragment screening methods, with examples for BRD4 and CREBBP. And while we’re on the topic of computational methods, Olgun Guvench of SilcsBio has a brief review in Drug Discov. Today on computational functional group mapping.

Rounding out target-focused reviews, Paramjit Arora and colleagues at New York University focus on protein-protein interactions (PPIs) in a Trends Pharm. Sci. paper. This covers multiple approaches to finding PPI inhibitors, including fragment-based, and also touches on hotspots and structure-based design.

Biophysics
It is impossible to imagine FBLD without biophysics, and this is the topic of an authoritative review in Nat. Rev. Drug Disc. by Jean-Paul Renaud (NovAliX), Chun-wa Chung (GlaxoSmithKline), U. Helena Danielson (Uppsala University), Ursula Egner (Bayer), Michael Hennig (leadXpro), Rod Hubbard (University of York) and Herbert Nar (Boehringer Ingelheim). In addition to covering all the major techniques, the paper does a great job of delving into some of the more obscure and emerging methods, providing an excellent discussion of the throughput and requirements for each technique as well as the kinds of information obtained. Although the review is broader than FBLD, the application of biophysical techniques to fragments is a major theme. The researchers also remind us that, “contrary to the belief that all drug discovery challenges are best solved through the introduction of new technologies, substantial advances can also be driven by innovative application.”

Individual biophysical techniques also received plenty of attention over the year, including three on NMR. The first, by Alvar Gossert and Wolfgang Jahnke (Novartis) in Prog. Nucl. Magn. Reson. Spectrosc., is a 44-page practical guide to identifying and validating protein ligands. This contains a wealth of information on most of the NMR methods you will ever likely encounter; it includes a handy chart summarizing the molecular weight and concentration limits for each technique, suggested workflows, and thorough discussions of potential pitfalls. The review may appear daunting to the novitiate – it is replete with equations and pulse sequences – but the writing is clear. In the end, much comes down to the concept of the “validation cross”, a rubric for assessing the integrity of both ligand and protein, and evaluating binding effects on both ligand and protein.

Two additional reviews, both from William Pomerantz and colleauges at the University of Minnesota, focus specifically on protein-observed 19F NMR. The first, a Perspective in J. Med. Chem., is a good general introduction. Despite being the 13th most abundant element on our planet, only five natural products are confirmed to contain fluorine. Introducing this element into proteins – as has been done in more than 70 cases – can be a useful approach for discovering new ligands. And if you want to start doing this yourself, a paper in Nature Protocols provides practical details.

Turning to other biophysical techniques, surface plasmon resonance (SPR) continues to be very popular, and is reviewed by Alain Chavanieu and Partine Pugnière in Expert Opin. Drug Discov. The paper provides a good general overview on using SPR for FBLD, covering the theory, history, various screening strategies, comparison to other methods, recent applications to a variety of different targets, and a suggested workflow.

Calorimetry is less commonly used for fragment screening, even though it can provide thermodynamic data. Michael Recht and collaborators at the Palo Alto Research Center and Zenobia discuss both enthalpy arrays as well as more conventional isothermal titration calorimetry (ITC) in a Methods Enzymol. chapter.

Chemistry
But while biophysics is important, FBLD would be nowhere without chemistry. In MedChemComm, Stefan Kathman and Alexander Statsyuk (then Northwestern, now University of Houston) review one chemical approach, covalent tethering. This touches on the original reversible (thermodynamically-controlled) disulfide tethering approach developed back at Sunesis but is primarily focused on irreversible (kinetically-controlled) methods. The paper does an excellent job summarizing challenges, potential pitfalls, design rules, and recent successes. As of early this year the Statsyuk lab had sent their 100-member covalent fragment library to nine different research groups, three of which had already identified hits. The review ends with some provocative questions, and it will be fun for practitioners to answer them as covalent approaches garner increasing attention.

Another chemical technique we’ve touched on is substrate activity screening (SAS), and this is reviewed in ChemMedChem by Pieter Van der Veken and collaborators at the University of Antwerp. All published examples are summarized, including the modified approach developed by the Van der Veken lab; some unpublished data are also discussed. The paper also includes a good general section on the subtleties and complexities of transforming substrates into inhibitors.

Finally, if all this is a bit too much, a good general review on FBLD was published in Pharmacol. Ther. by Martin Scanlon and colleagues at Monash University. This concise but thorough paper covers theory, history, library design, hit finding and characterization, and select clinical success stories. The longest section is devoted to chemical strategies for elaborating fragments, and includes some of the less commonly used methods such as target-guided synthesis, Tethering, and off-rate screening.

And that’s it for this year. Thanks for reading, and especially for commenting. Take care, do important work, and may 2017 be better than we can reasonably hope.

13 May 2015

When Fragments don't deliver...

In the olden days (1980s), during the cold war, Russia was "a riddle wrapped in a mystery inside an enigma".  Kremlin Watching was serious and important thing. When I write up papers, I do the same thing but trying to figure out what the actual story is.  We all know a lot more happened than is written down in 10-20 pages of an article.  This paper has me really doing it; so follow along.

Tuberculosis is a scourge caused by a mighty nasty bug.  People have been using fragments to try to combat it for a long time: 2009 and 2014: targeting pantothenate synthesis and biotin synthesis. AstraZeneca join the party (just as Entasis spins out) with this paper.  In it, they describe their NMR fragment screen combined with a HTS biochemical screen targeting thymidine synthesis.  All the TK inhibitors are TMP or thymidine analogs.  The HTS of 120,000 compounds lead to multiple 1-30 uM active site binding (confirmed by HSQC NMR) inhibitors.  Compound 1
Cpd 1.  3.6 uM, 0.46 LE, 3.54 LLE.  
Figure 2.
was chosen as the basis for the hit to lead campaign.  Modeling suggested that the pyridone core is a thymidine mimic (Figure 2). This novel core allowed to reach sub micromolar potency within 10 compounds of the original hit.  The pyrimidine core was also potent, but not as much as the pyridone.  Pyranones were inactive, as was any other group but the cyano at the 2 position. Crystallography was a key to verifying the binding mode of the compounds.  One point of this is that verified means within 1 A of the predicted pose.  SAR led to the fused pyridinone, a 2 nM inhibitor, which nonetheless had no cellular activity.  The propose that this is due to the ionic nature of the compound, but ureas, amides, and sulfonamides did not afford the desired activity. 
Figure 3.  Fused Pyridinone showing X-ray Contacts

So, as is becoming a very common theme in fragments, they decided to use fragments to try to discover an alternate scaffold.  Using TROSY (HSQC for big proteins), they screen 1200 fragments in pools of 6.  Those fragment hits, termed FRITs which is a first for me (I think I like it.), with a LE greater than 0.25 were followed up by X-ray crystallography.
Figure 4.  Napthyridinone FRIT.  590 uM, LE=0.3. 
Figure 4. shows the best FRIT and its crystal contacts.  Combining this with the knowledge from the cyanopyridinone series, a virtual library was created and docked.  Hidden in their description, it appears that the library was passed by real chemists to prioritize the cpds.  Kudos.  With very limited SAR, they achieved significant potency (Figure 5), but still without cellular potency. 
Figure 5. 200 nM, LE=0.34.  

But, WAIT, this series wasn't advanced any further because the cyanopyridinone was in "advanced lead generation".  Why, you ask?  Well, the oxidized form of Cpd 1 had exhibited moderate cellular activity.  While they don't say it, I would imagine that this means that in doing the analytical work on the compound they found a portion that had oxidized, cleaned it up, and then tested the "bad" part.  I would love to know if this is how it happened.  I would hate to learn they had planned on an oxidized compound all along.

So, on to sulfone and sulfoxides of Cpd 1.  Knowledge from the cyanopyridinone series was used to select appropriate substituents, which seems to indicate a timeline of how things happened or a "we've got nothing left to try" issue.  Again, I would love to know which.  Both the sulfones and sulfoxides showed cellular activity with increase in IC50.  And again X-ray showed that the binding mode was retained, with the sulfoxide adjacent to Arg95.  This then caused them to go back and look at the cyanopyridinones again and realize that the sulfone/sulfoxides might have just the right physicochemical properties.

I think this is a really good paper, and hopefully indicates that more work on this target and with these series are coming.So, I don't know if the fragments failed, or if something better came along.  I would think the latter, but it could be the former.  Again, I would love to know.