Chemistry 125: Lecture 28 November 8, 2010 Communicating Molecular Structure in Diagrams and Words Correct configuration is vital in drug molecules, like eribulin. It is important that chemists agree on notation and nomenclature in order to communicate molecular constitution and configuration. Clear notation also aids clarity of thought. The conventional 1891 Fischer projection, which has been indispensable in understanding sugar configurations for over a century, was invented in order to count stereoisomers. Ambiguity in diagrams or words has led to multibillion dollar patent disputes involving popular pharmaceuticals. International agreements provide descriptive, unambiguous, unique, systematic “IUPAC” names that are reasonably convenient for most organic molecules of modest molecular weight. Also in 1891 Fischer devised the D,L “genealogical” scheme to describe relative configurations, but it can be cumbersome or ambiguous. Preliminary For copyright notice see final page of this file Halichondrin B: A Marine Natural Product with Potent In Vitro and In Vivo Antitumor Activity Discovery of E7389 Starting From the Halichondrin B C.1-C.38 Macrolide HO O HO H H Active Fragment of Halichondrin B Structure-Activity Relationship Study Me O O O O O O Me O O OMe OH H2N H O O H 19 “stereogenic centers” O O H SAR Version of Active Fragment became Drug Candidate E7389, now “Eribulin” halichondrin B C.1-C.38 macrolide H"Simplified" H O O H O H O O Me O H O E7389 "In Vitro and In Vivo Anticancer Activities of Synthetic Macrocyclic Ketone Analogues of Halichondrin B" M.J. Towle, K.A. Salvato, J. Budrow, B.F. Wels, G. Kuznetsov, K.K. Aalfs, S. Welsh, W. Zheng, B.M. Seletsky, M.H. Palme, G.J. Habgood, L.A. Singer, L.V. DiPietro, Y.Wang, J.J. Chen, D.A. Quincy, A.Davis K. Yoshimatsu, Y. Kishi, M.J. Yu, and B.A. Littlefield, Cancer Res., February 1, 2001; 61(3): 1013-1021 219 > 500,000 configurational isomers! ClinicalTrials.gov currently has 98,100 trials with locations in 174 countries. (Nov. 3, 2010) E7389 Phase III Nov 2008 (Nov. 2009) (Nov. 3, 7, 2010) 2008) Lipitor A $10,000,000,000 Problem in Stereochemical Notation The world’s best selling drug ($10.86 billion in 2004) Oct. 12, 2005 NEW YORK - Pfizer Inc. won a significant victory on Wednesday when a British judge upheld a key patent covering its blockbuster cholesterol drug Lipitor in the United Kingdom but the medication still faces a similar yet more important case in the United States. (Analogus decision 8/2/2006 in U.S. Court of Appeals) Judge Nicholas Pumfrey upheld the patent covering atorvastatin, Lipitor’s active ingredient, but ruled that another patent was invalid. Indian pharmaceutical company Ranbaxy Laboratories Ltd. had challenged both patents, and was joined by Britain’s Arrow Generics Ltd. against the second patent that was ruled invalid. Pfizer said the decision upholding the exclusivity of the patent covering atorvastatin until November 2011 was an important victory for scientists. What is Patented? single enantiomer (Lipitor, drawn in figure) … or racemate (described in text) F - (CH2)2 OH O Ca+2 O H-N i-Pr Number of permutations much greater than the total number of protons, neutrons, and electrons in the Solar system! Opinion of Sir Nicholas Pumfrey In the '633 patent, it is absolutely clear from context throughout that formula (I) is being used to denote a racemate. In my judgment, every time the skilled person sees formula I or formula X he will see it with eyes that tell him that in that racemate, there is a single enantiomer that is the effective compound, and that he can resolve the racemate using conventional techniques to extract that enantiomer. When one comes to claim 1, which echoes the purpose of the invention with its conventional reference to pharmaceutically Pfizer’s latertopatent acceptable salts, he will, in myThus judgment, continue see the formulae in this light. on the single enantiomer In my view, the claim is an invalid repeat, and covers the racemate and patent protection will run the individual enantiomers. out three years earlier ! I X Constitutional Nomenclature Conventions Geneva (1892) IUPAC, International Union of Pure & Applied Chemistry http://www.chem.qmw.ac.uk/iupac/ http://acdlabs.com/iupac/nomenclature Formal name should be: • Clearly Descriptive • Unambiguous • Composition, Constitution, Configuration, Conformation i.e. Stereochemistry Unfortunately "Amide" means One name one structure both R2N and RCONH2 Eisai graphics Unique Indexing Alternatives: composition, computer Research One structure one name • Manageable Institute (e.g. Quick, Easy, Short, Pronounceable) Eribulin Systematic Constitutional Nomenclature bromo Choose the “Main Chain”methyl for Greek Root Name • Longest • Most Substituents (to give simpler names) Number the Chain Atoms methyl Br 6 7 3 2 1 5 4 chloro Cl 2 ethyl 1 7-bromo-2-chloro-3-ethyl-6,7-dimethylnonane ? Br • Lowest number at First Difference Name Substituents 3 Cl (1-chloroethyl) octane Br Alphabetize (& Count) Cl http://acdlabs.com/iupac/nomenclature/93/r93_338.htm WOW! ) ( [ ] Thank God for pictures and computer graphics. Some Useful Non-Systematic Names Isopentane Isobutane X X Neopentane X X Isopropyl sec-Butyl tert-Butyl Neopentyl Nomenclature Drill available on course website. Configurational Nomenclature Phenomenological d/l +/- Relative D/L Absolute R/S Configurational Nomenclature m.p. [a]D 140°C 0° (meso) 170°C +13° (dextro +) 170°C -13° (laevo -) Phenomenological Tartaric Acid Isomers Genealogical (Fischer, 1891) D-Tartaric Acid Relative (by synthesis) to HOCH2CH(OH)CHO d-(+)-glyceraldehyde Defined as “D”-glyceraldehyde (Fischer’s Guess) Multi-Step Synthesis First of 210 Tables Glyceraldehyde D D Lactic Acid (1978) Paul D. Bartlett age 24 Problem for Monday: Consider HOMO/LUMO alternatives during the reaction of HI with 1,3-butanediol to give 4-iodo-2-butanol >2000 Compounds in the 210 Tables 24 years old Absolute Configuration J. M. Bijvoet van't Hoff Laboratory, Univ. Utrecht (1949-51) Na Rb d-(L)-Tartrate X-ray anomalous dispersion 60 year old Fischer Guess for of our “The question of nomenclature is beyond the scope investigation... The problem of nomenclature (L)-Tartrate now concerns given configurations, and requires a notation which denotes these configurations in an unambiguous and if possible selfexplanatory way.” (Bijvoet, 1951) Naming Double Bond Configuration Malic Acid (HO2C)CH(OH).CH2. (CO2H) D (HO2C)HC=CH(CO2H) Maleic & Fumaric Acids Absolute nomenclature is hard to generalize (though relative is fine) H3 C cis CH3 H H COOH cis or trans? H H COOH D HOOC O + H2O O cis COOH O (on this side of) HOOC H trans (across) Double Bond Configuration Assign groups at either end "priority" by atomic number (or weight for isotopes) at first difference H H3C H C CH3 H O C COOH O H HO O HO O O C COOH O H3C H H H C CH3 H The names trans and cis are "polluted" previous usage. (E)ntgegen (Opposed) (Z)by usammen (Together) In Assigning Priority Proceed One "Shell" at a Time (respecting previous decisions) O H O C Win O Cl is high Tie C H O H H in priority, but irrelevant; H the decision Cl is already made. H3 C O Win C O Tie H C C H Cl R. S. Cahn V. C. K. Ingold Prelog R. Robinson by permission J. D. Roberts The 1950s "CIP" Priority Scheme is Conventional R. B.Woodward Robinson: "Hello Katchalsky. What are you doing here in Zurich?" Prelog: "Excuse me, Sir Robert, I am only Prelog, and I live here." Robinson: "You know, Prelog, your and Ingold's configurational notation is all wrong." Prelog: "Sir Robert, it can't be wrong. It is just a convention. You either accept it or not." Robinson: "Well then, if it is not wrong, it is absolutely unnecessary." from V. Prelog, My 132 semesters of chemistry studies (1981) http://www.bl.uk/onlinegallery/themes/euromanuscripts/lindisfarne.html Exercise for Monday: Eadfrith’s Error (Click here & create your very own chiral conventions) D H HO left turn 1 CIP (R/S) Nomenclature CH3 for Stereogenic Centers HO 2 2 CH3 2 D3 HO H4 (S)inister (left) H HO OH 3 H D right turn CH3 COOH 4 CH3 1 H 1 HO H4 D3 (R)ectus (right) COOH H (2R,3R)2,3-dihydroxy butanedioic acid H Bloomer Gate Organic End of Lecture 28 Nov. 8, 2010 Copyright © J. M. McBride 2009,2010. Some rights reserved. Except for cited third-party materials, and those used by visiting speakers, all content is licensed under a Creative Commons License (Attribution-NonCommercial-ShareAlike 3.0). Use of this content constitutes your acceptance of the noted license and the terms and conditions of use. Materials from Wikimedia Commons are denoted by the symbol . Third party materials may be subject to additional intellectual property notices, information, or restrictions. The following attribution may be used when reusing material that is not identified as third-party content: J. M. McBride, Chem 125. License: Creative Commons BY-NC-SA 3.0