Organic Chemistry Second Edition David Klein Chapter 14 Ethers and Epoxides; Thiols and Sulfides Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. Klein, Organic Chemistry 2e 14.1 Introduction to Ethers • An ether group includes an oxygen atom that is bonded to TWO –R groups • -R groups can be alkyl, aryl, or vinyl groups • Would the compound below be considered an ether? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-2 Klein, Organic Chemistry 2e 14.1 Introduction to Ethers • Compounds containing ether groups are quite common Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-3 Klein, Organic Chemistry 2e 14.2 Naming Ethers • Common names are used frequently 1. Name each –R group 2. Arrange them alphabetically 3. End with the word, “ether” Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-4 Klein, Organic Chemistry 2e 14.2 Naming Ethers • IUPAC systematic names are often used as well 1. Make the larger of the –R groups the parent chain 2. Name the smaller of the –R groups as an alkoxy substituent • Practice with SkillBuilder 14.1 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-5 Klein, Organic Chemistry 2e 14.2 Naming Ethers • Name the following molecule • Draw the structure for (R)-1-methoxycyclohexen-3-ol Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-6 Klein, Organic Chemistry 2e 14.3 Structure and Properties of Ethers • The bond angle in ethers is very similar to that found in water and in alcohols • Is the oxygen atom in an ether sp3, sp2, or sp hybridized? • How do the –R groups affect the bond angle? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-7 Klein, Organic Chemistry 2e 14.3 Structure and Properties of Ethers • In chapter 13, we learned that due to H-bonding, alcohols have relatively high boiling points • What is the maximum number of H-bonds an alcohol can have? • Draw an H-bond between an ether and an alcohol • What is the maximum number of H-bonds an ether can have? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-8 Klein, Organic Chemistry 2e 14.3 Structure and Properties of Ethers • In chapter 13, we learned that due to H-bonding, alcohols have relatively high boiling points • Would you expect the boiling point of an ether to be elevated similar to alcohols? • WHY or WHY not? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-9 Klein, Organic Chemistry 2e 14.3 Structure and Properties of Ethers • Explain the boiling point trends below using all relevant intermolecular attractions – Trend 1 – Trend 2 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-10 Klein, Organic Chemistry 2e 14.3 Structure and Properties of Ethers • Ethers are often used by organic chemists as solvents – Relatively low boiling points allow them to be evaporated after the reaction is complete – Their dipole moment allows them to stabilize charged or partially charged transition states. HOW? – They are NOT protic. WHY is that an advantage for a solvent in many reactions? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-11 Klein, Organic Chemistry 2e 14.4 Crown Ethers • Metal atoms with a full or partial positive charge can be stabilized by ether solvents • Ethers are generally used as the solvent in the Grignard reaction • Give another reason why an ether makes a good solvent in this reaction Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-12 Klein, Organic Chemistry 2e 14.4 Crown Ethers • Crown ethers have been shown to form especially strong attractions to metal atoms. WHY? • Note how many carbon atoms separate the oxygens • Why are they called CROWN ethers? • Explain the numbers found in their names Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-13 Klein, Organic Chemistry 2e 14.4 Crown Ethers • The size of the metal must match the size of the crown to form a strong attraction • 18-crown-6 fits a K+ ion just right Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-14 Klein, Organic Chemistry 2e 14.4 Crown Ethers • Normally metal ions are not soluble in low polarity solvents. WHY? • The crown ether – metal complex should dissolve nicely in low polarity solvents. WHY? • Imagine how a crown ether could be used to aid reactions between ion (especially anions) and low polarity organic substrates Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-15 Klein, Organic Chemistry 2e 14.4 Crown Ethers • The F- ion below is ready to react because the K+ ion is sequestered by the crown ether • Without the crown ether, the solubility of KF in benzene is miniscule Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-16 Klein, Organic Chemistry 2e 14.4 Crown Ethers • Generally, F- ion is not used as a nucleophile, because it is strongly solvated by polar solvents • Such solvation greatly reduces its nucleophilic strength • In the presence of the crown ether, it is soluble enough in a nonpolar solvent that it can readily attack an electrophile Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-17 Klein, Organic Chemistry 2e 14.4 Crown Ethers • Smaller crown ethers bind smaller cations • Practice with conceptual checkpoint 14.4 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-18 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • Diethyl ether is prepared industrially by the acidcatalyzed dehydration of ethanol • How is it a dehydration? • Can this method be used to make asymmetrical ethers? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-19 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • The Williamson ether synthesis is a viable approach for many asymmetrical ethers • What happens to the halide? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-20 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • The Williamson ether synthesis is a viable approach for many asymmetrical ethers • The alkoxide that forms in step 1 is also a strong base • Are elimination products likely for methyl, primary, secondary, or tertiary alkyl halides? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-21 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • Use the Williamson ether approach to prepare MTBE • Consider a retrosynthetic disconnect on the t-butyl side • It is better to make your retrosynthetic disconnect on the methyl side. WHY? • Practice with SkillBuilder 14.2 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-22 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • Use the Williamson ether approach to synthesize the following molecule Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-23 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • Recall from section 9.5 that oxymercurationdemercuration can be used to synthesize alcohols • Is the addition Markovnikov or anti-Markovnikov? • Is the addition syn or anti? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-24 Klein, Organic Chemistry 2e 14.5 Preparation of Ethers • Similarly, alkoxymercuration-demercuration can be used to synthesize ethers • Is the addition Markovnikov or anti-Markovnikov? • Is the addition syn or anti? • Practice conceptual checkpoints 14.8–14.10 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-25 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • As we mentioned earlier, because they are aprotic, ethers are generally unreactive • However, ethers can react under the right conditions • Consider the ether below • Where are the most reactive sites? • Is it most likely to react as an acid, base, nucleophile, electrophile, etc.? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-26 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • Ethers can undergo acid-promoted cleavage Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-27 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • Draw a complete mechanism and predict the products for the following acid-promoted cleavage Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-28 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • To promote cleavage, HI and HBr are generally effective • HCl is less effective, and HF does not cause significant cleavage • Explain the trend above considering the relative strength of the halide nucleophiles • Why is the cleavage considered acid-promoted rather than acid-catalyzed? • Practice with conceptual checkpoint 14.11 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-29 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • Predict products for the reaction below, and draw a complete mechanism Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-30 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • Recall from section 11.9 that ethers can undergo autooxidation • Hydroperoxides can be explosive, so laboratory samples of ether must be frequently tested for the presence of hydroperoxides before they are used • The autooxidation occurs through a free radical mechanism – see next few slides Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-31 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-32 Klein, Organic Chemistry 2e 14.6 Reactions of Ethers • Recall that the net reaction is the sum of the propagation steps Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-33 Klein, Organic Chemistry 2e 14.7 Naming Epoxides • For cyclic ethers, the size of the ring determines the parent name of the molecule • Oxiranes are also known as epoxides • Which cyclic ether system do you think is most reactive? WHY? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-34 Klein, Organic Chemistry 2e 14.7 Naming Epoxides • An epoxide can have up to 4 –R groups • Although they are unstable, epoxides are found commonly in nature Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-35 Klein, Organic Chemistry 2e 14.7 Naming Epoxides • There are two methods for naming epoxides 1. The oxygen is treated as a side group, and two numbers are given as its locants 2. Oxirane is used as the parent name Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-36 Klein, Organic Chemistry 2e 14.7 Naming Epoxides • Name the molecules below by both methods if possible • Practice conceptual checkpoints 14.12 and 14.13 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-37 Klein, Organic Chemistry 2e 14.8 Preparation of Epoxides • Recall from section 9.9 that epoxides can be formed when an alkene is treated with a peroxy acid • MCPBA and peroxyacetic acid are most commonly used Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-38 Klein, Organic Chemistry 2e 14.8 Preparation of Epoxides • Recall that the process is stereospecific Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-39 Klein, Organic Chemistry 2e 14.8 Preparation of Epoxides • • • • Epoxides can also be formed from halohydrins What is a halohydrin? How are halohydrins formed from alkenes? When a Halohydrin is treated with NaOH, a ring-closing reaction can occur Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-40 Klein, Organic Chemistry 2e 14.8 Preparation of Epoxides Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-41 Klein, Organic Chemistry 2e 14.8 Preparation of Epoxides • Assess the overall stereochemistry of the epoxidation that occurs through the halohydrin intermediate • Practice with SkillBuilder 14.3 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-42 Klein, Organic Chemistry 2e 14.9 Enantioselective Epoxidation • The epoxidation methods we have discussed so far are NOT enantioselective • Draw the products racemic mixture Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-43 Klein, Organic Chemistry 2e 14.9 Enantioselective Epoxidation • The epoxidation forms a racemic mixture, because the flat alkene can react on either face Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-44 Klein, Organic Chemistry 2e 14.9 Enantioselective Epoxidation • To be enatioselective at least one of the reagents (or catalyst) in a reaction must be chiral • The Sharpless catalyst forms such a chiral complex with an allylic alcohol Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-45 Klein, Organic Chemistry 2e 14.9 Enantioselective Epoxidation • The desired epoxide can be formed if the right catalyst is chosen. Note the position of the –OH group • How does the catalyst favor just one epoxide product? • Practice with conceptual checkpoint 14.16 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-46 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Because of their significant ring strain, epoxides have great synthetic utility as intermediates • Propose some reagents that might react with an epoxide to provide a specific functional group • Propose some reagents that might react with an epoxide to alter the carbon skeleton Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-47 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Strong nucleophiles react readily with epoxides • Predict whether each step is product or reactant favored, and explain WHY Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-48 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • In general, alkoxides are not good leaving groups • The ring strain associated with the epoxide increases its potential energy making it more reactive– see the energy diagram on the next slide Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-49 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • The epoxide reaction is both more kinetically and more thermodynamically favored. WHY? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-50 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Epoxides can be opened by many other strong nucleophiles as well • Both regioselectivity and stereoselectivity must be considered – see next few slides Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-51 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Given that the epoxide ring-opening is SN2, predict the outcome of the following reactions • Pay attention to regio- and stereoselectivity. EXPLAIN WHY • Practice with SkillBuilder 14.4 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-52 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Acidic conditions can also be used to open epoxides Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-53 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Water or an alcohol can also be used as the nucleophile under acidic conditions • Predict the products and draw a complete mechanism • Antifreeze (ethylene glycol) is made industrially by this method Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-54 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • Propose an explanation for the following regiochemical observations • Consider both steric and electronic effects (induction) Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-55 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • If the nucleophile preferentially attacks the tertiary carbon under acidic conditions, is the mechanism likely SN1 or SN2? • Considering the observations below, is the mechanism likely SN1 or SN2? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-56 Klein, Organic Chemistry 2e 14.10 Ring-opening of Epoxides • When the nucleophile attacks a tertiary center of the epoxide, the intermediate it attacks takes on some carbocation character (SN1), but not completely • Give reaction conditions for the following reaction • Practice with SkillBuilder 14.5 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-57 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Sulfur appears just under oxygen on the periodic table • Sulfur appears in thiols as an –SH group analogous to the –OH group in alcohols • The name of a compound with an –SH group ends in “thiol” rather than “ol” • Note that the “e” of butane is not dropped in the name of the thiol Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-58 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Thiols are also known as mercaptans • The –SH group can also be named as part of a side group rather than as part of the parent chain • The mercaptan name comes from their ability to complex mercury • 2,3-dimercapto-1-propanol is used to treat mercury poisoning. WHY? Draw its structure Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-59 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Thiols are known for their unpleasant odor • Skunks use thiols as a defense mechanism • Methanethiol is added to natural gas (methane) so that gas leaks can be detected • Your nose is a very sensitive instrument • The hydrosulfide ion (HS-) is a strong nucleophile and a weak base • HS- promotes SN2 rather than E2 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-60 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Predict the outcome of the following reactions, and draw a complete mechanism • Practice with conceptual checkpoint 14.22 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-61 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Thiols have a pKa of about 10.5 • Recall that water has a pKa of 15.7 • Predict whether the equilibrium below will favor products or reactants and draw the mechanism thiolate ion • Thiolates are excellent nucleophiles Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-62 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • A thiolate can attack Br2 to produce a disulfide • How does the oxidation number change? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-63 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Disulfides can be reduced by the reverse reaction • The interconversion between thiol and disulfide can also occur directly via a free radical mechanism. Propose a mechanism • The bond dissociation energy of a S-S bond is only about 53 kcal/mol. WHY is that significant? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-64 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Sulfur analogs of ethers are called sulfides or thioethers • Sulfides can also be named as a side group Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-65 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Sulfides are generally prepared by nucleophilic attack of a thiolate on an alkyl halide • How are thiolates generally prepared? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-66 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Sulfides undergo a number of reactions 1. Attack on an alkyl halide – The process produces a strong alkylating reagent that can add an alkyl group to a variety of nucleophiles Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-67 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides 2. Sulfides can also be oxidized • Sodium meta-periodiate can be used to form the sulfoxide Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-68 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides 2. Sulfides can also be oxidized • Hydrogen peroxide can be used to give the sulfone Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-69 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • • Sulfoxides and sulfones have very little double bond character Which resonance contributor for each is the major contributor, and WHY? Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-70 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • • Because sulfides are readily oxidized, they make good reducing agents Recall the ozonolysis reaction from section 9.11 • Practice with conceptual checkpoint 14.23 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-71 Klein, Organic Chemistry 2e 14.11 Thiols and Sulfides • Predict any products or necessary reagents in the reaction sequence below • Verify the formal charge on the sulfur in the final product above Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-72 Klein, Organic Chemistry 2e 14.12 Synthetic Strategies Involving Epoxides • Epoxides can be used to install functional groups on adjacent carbons • Give necessary reagents for the reaction below • Practice with SkillBuilder 14.6 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-73 Klein, Organic Chemistry 2e 14.12 Synthetic Strategies Involving Epoxides • By reacting an epoxide with a Grignard reagent, the carbon skeleton can be modified • You may think of an epoxide as the starting material Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-74 Klein, Organic Chemistry 2e 14.12 Synthetic Strategies Involving Epoxides • An epoxide can be used to install a two carbon chain between an R group and an OH group • Recall that a carbonyl can be used to install a one carbon chain between an R group and an OH group Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-75 Klein, Organic Chemistry 2e 14.12 Synthetic Strategies Involving Epoxides • Give necessary reagents for the reaction below • Practice with SkillBuilder 14.7 Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-76 Klein, Organic Chemistry 2e Additional Practice Problems • Name the following molecule • Draw the structure for (4-methylcyclohexyl)phenylether Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-77 Klein, Organic Chemistry 2e Additional Practice Problems • Fill in the missing intermediates and reagents in the scheme below Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-78 Klein, Organic Chemistry 2e Additional Practice Problems • Fill in the missing intermediates and reagents in the scheme below Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-79 Klein, Organic Chemistry 2e Additional Practice Problems • Give necessary reagents to complete the synthesis below Copyright © 2015 John Wiley & Sons, Inc. All rights reserved. 14-80 Klein, Organic Chemistry 2e