Catalytic Enantioselective Carbonyl Allylation and Propargylation via Alcohol-Mediated Hydrogen Transfer: Merging the Chemistry of Grignard and Sabatier.

Merging the characteristics of transfer hydrogenation and carbonyl addition, we have developed a new class of catalytic enantioselective C-C bond formations. In these processes, hydrogen transfer between alcohols and π-unsaturated reactants generates carbonyl-organometal pairs that combine to deliver products of addition. On the basis of this mechanistic paradigm, lower alcohols are converted directly to higher alcohols in the absence of premetalated reagents or discrete alcohol-to-carbonyl redox reactions. In certain cases, due to a pronounced kinetic preference for primary versus secondary alcohol dehydrogenation, diols and higher polyols are found to engage in catalytic stereo- and site-selective C-C bond formation-a capability that further enhances efficiency by enabling skeletal construction events without extraneous manipulations devoted to the installation and removal of protecting groups. While this Account focuses on redox-neutral couplings of alcohols, corresponding aldehyde reductive couplings mediated by 2-propanol were developed in parallel for most of the catalytic transformations reported herein. Mechanistically, two distinct classes of alcohol C-H functionalizations have emerged, which are distinguished by the mode of pronucleophile activation, specifically, processes wherein alcohol oxidation is balanced by (a) π-bond hydrometalation or (b) C-X bond reductive cleavage. Each pathway offers access to allylmetal or allenylmetal intermediates and, therefrom, enantiomerically enriched homoallylic or homopropargylic alcohol products, respectively. In the broadest terms, carbonyl addition mediated by premetalated reagents has played a central role in synthetic organic chemistry for well over a century, but the requisite organometallic reagents pose issues of safety, require multistep syntheses, and generate stoichiometric quantities of metallic byproducts. The concepts and catalytic processes described in this Account, conceived and developed wholly within the author's laboratory, signal a departure from the use of stoichiometric organometallic reagents in carbonyl addition. Rather, they reimagine carbonyl addition as a hydrogen autotransfer process or cross-coupling in which alcohol reactants, by virtue of their native reducing ability, drive the generation of transient organometallic nucleophiles and, in doing so, serve dually as carbonyl proelectrophiles. The catalytic allylative and propargylative transformations developed to date display capabilities far beyond their classical counterparts, and their application to the total synthesis of type-I polyketide natural products have evoked a step-change in efficiency. More importantly, the present data suggest that diverse transformations traditionally reliant on premetalated reagents may now be conducted catalytically without stoichiometric metals. This Account provides the reader and potential practitioner with a catalog of enantioselective alcohol-mediated carbonyl additions-a user's guide, 10-year retrospective, and foundation for future work in this emerging area of catalytic C-C bond formation.

[1]  M. Krische,et al.  Enantioselective Formation of CF3-Bearing All-Carbon Quaternary Stereocenters via C-H Functionalization of Methanol: Iridium Catalyzed Allene Hydrohydroxymethylation. , 2017, Journal of the American Chemical Society.

[2]  S. W. Kim,et al.  Asymmetric Allylation of Glycidols Mediated by Allyl Acetate via Iridium-Catalyzed Hydrogen Transfer. , 2017, Organic letters.

[3]  Pradeep Kumar,et al.  Transition metal catalysis-a unique road map in the stereoselective synthesis of 1,3-polyols. , 2017, Organic & biomolecular chemistry.

[4]  G. Chelucci Metal-catalyzed dehydrogenative synthesis of pyrroles and indoles from alcohols , 2017 .

[5]  Sheng-rong Guo,et al.  Recent Advances of Oxidative Radical Cross‐Coupling Reactions: Direct α‐C(sp3)–H Bond Functionalization of Ethers and Alcohols , 2017 .

[6]  M. Krische,et al.  Metal-catalyzed reductive coupling of olefin-derived nucleophiles: Reinventing carbonyl addition , 2016, Science.

[7]  M. Krische,et al.  Enantioselective Formation of All-Carbon Quaternary Centers via C-H Functionalization of Methanol: Iridium-Catalyzed Diene Hydrohydroxymethylation. , 2016, Journal of the American Chemical Society.

[8]  Jean Rodriguez,et al.  Catalytic enantioselective OFF ↔ ON activation processes initiated by hydrogen transfer: concepts and challenges. , 2016, Chemical communications.

[9]  M. Krische,et al.  C-Propargylation Overrides O-Propargylation in Reactions of Propargyl Chloride with Primary Alcohols: Rhodium-Catalyzed Transfer Hydrogenation. , 2016, Angewandte Chemie.

[10]  M. Krische,et al.  Iridium-Catalyzed C—C Coupling of a Simple Propargyl Ether with Primary Alcohols: Enantioselective Homoaldol Addition via Redox-Triggered (Z)-Siloxyallylation. , 2016 .

[11]  S. Oda,et al.  Ruthenium-Catalyzed Transfer Hydrogenation for C–C Bond Formation: Hydrohydroxyalkylation and Hydroaminoalkylation via Reactant Redox Pairs , 2016, Topics in Current Chemistry.

[12]  Jiajie Feng,et al.  Enantioselective Alcohol C-H Functionalization for Polyketide Construction: Unlocking Redox-Economy and Site-Selectivity for Ideal Chemical Synthesis. , 2016, Journal of the American Chemical Society.

[13]  M. Krische,et al.  Ruthenium-BINAP Catalyzed Alcohol C-H tert-Prenylation via 1,3-Enyne Transfer Hydrogenation: Beyond Stoichiometric Carbanions in Enantioselective Carbonyl Propargylation. , 2016, Journal of the American Chemical Society.

[14]  Fei Huang,et al.  C-Alkylation of Ketones and Related Compounds by Alcohols: Transition-Metal-Catalyzed Dehydrogenation. , 2016, Angewandte Chemie.

[15]  M. Krische,et al.  Asymmetric Iridium-Catalyzed C-C Coupling of Chiral Diols via Site-Selective Redox-Triggered Carbonyl Addition. , 2016, Topics in current chemistry.

[16]  Jean Rodriguez,et al.  A Step into an eco-Compatible Future: Iron- and Cobalt-catalyzed Borrowing Hydrogen Transformation. , 2016, ChemSusChem.

[17]  V. Landge,et al.  Transition-Metal-Catalyzed Hydrogen-Transfer Annulations: Access to Heterocyclic Scaffolds , 2015 .

[18]  M. Krische,et al.  Ruthenium Catalyzed Diastereo- and Enantioselective Coupling of Propargyl Ethers with Alcohols: Siloxy-Crotylation via Hydride Shift Enabled Conversion of Alkynes to π-Allyls. , 2015, Journal of the American Chemical Society.

[19]  M. Krische,et al.  Diastereo- and Enantioselective Iridium Catalyzed Carbonyl (α-Cyclopropyl)allylation via Transfer Hydrogenation. , 2015, Chemistry.

[20]  M. Krische,et al.  Enantioselective Ruthenium‐Catalyzed Carbonyl Allylation via Alkyne—Alcohol C—C Bond‐Forming Transfer Hydrogenation: Allene Hydrometalation vs. Oxidative Coupling. , 2015 .

[21]  Matthew N. Grayson,et al.  Ruthenium-Catalyzed Asymmetric Hydrohydroxyalkylation of Butadiene: The Role of the Formyl Hydrogen Bond in Stereochemical Control. , 2015, Journal of the American Chemical Society.

[22]  M. Krische,et al.  Diastereo- and Enantioselective Iridium Catalyzed Coupling of Vinyl Aziridines with Alcohols: Site-Selective Modification of Unprotected Diols and Synthesis of Substituted Piperidines. , 2015, Journal of the American Chemical Society.

[23]  R. Saicic Corrigendum to “Protecting group-free syntheses of natural products and biologically active compounds” [Tetrahedron 70 (2014) 8183–8218] , 2015 .

[24]  M. Krische,et al.  Paraformaldehyde and Methanol as C1 Feedstocks in Metal‐Catalyzed C—C Couplings of π‐Unsaturated Reactants: Beyond Hydroformylation , 2015 .

[25]  Qin Yang,et al.  Substitution of alcohols by N-nucleophiles via transition metal-catalyzed dehydrogenation. , 2015, Chemical Society reviews.

[26]  M. Krische,et al.  Enantioselective ruthenium-catalyzed carbonyl allylation via alkyne-alcohol C-C bond-forming transfer hydrogenation: allene hydrometalation vs oxidative coupling. , 2015, Journal of the American Chemical Society.

[27]  M. Krische,et al.  Catalytic Enantioselective C—H Functionalization of Alcohols by Redox‐Triggered Carbonyl Addition: Borrowing Hydrogen, Returning Carbon , 2014 .

[28]  R. Saicic Protecting Group-Free Syntheses of Natural Products and Biologically Active Compounds , 2014 .

[29]  M. Krische,et al.  Catalyst-directed diastereo- and site-selectivity in successive nucleophilic and electrophilic allylations of chiral 1,3-diols: protecting-group-free synthesis of substituted pyrans. , 2014, Chemistry.

[30]  M. Krische,et al.  Alkynes as Allylmetal Equivalents in Redox-Triggered C–C Couplings to Primary Alcohols: (Z)-Homoallylic Alcohols via Ruthenium-Catalyzed Propargyl C–H Oxidative Addition , 2014, Journal of the American Chemical Society.

[31]  Jiajie Feng,et al.  Redox-Triggered C–C Coupling of Alcohols and Vinyl Epoxides: Diastereo- and Enantioselective Formation of All-Carbon Quaternary Centers via tert-(Hydroxy)-Prenylation , 2014, Journal of the American Chemical Society.

[32]  Jeremy R. Duvall,et al.  Catalytic asymmetric allylation of carbonyl compounds and imines with allylic boronates , 2014 .

[33]  M. Krische,et al.  Polyketide construction via hydrohydroxyalkylation and related alcohol C-H functionalizations: reinventing the chemistry of carbonyl addition. , 2014, Natural product reports.

[34]  M. Krische,et al.  Asymmetric alcohol C-H allylation and syn-crotylation: C9-C20 of tetrafibricin. , 2014, Organic letters.

[35]  M. Yus,et al.  Diastereoselective Allylation of Carbonyl Compounds and Imines: Application to the Synthesis of Natural Products , 2013 .

[36]  M. Krische,et al.  Ruthenium catalyzed reductive coupling of paraformaldehyde to trifluoromethyl allenes: CF3-bearing all-carbon quaternary centers. , 2013, Organic letters.

[37]  M. Krische,et al.  Chiral‐Anion‐Dependent Inversion of Diastereo‐ and Enantioselectivity in Carbonyl Crotylation via Ruthenium‐Catalyzed Butadiene Hydrohydroxyalkylation. , 2013 .

[38]  M. Krische,et al.  Iridium‐Catalyzed Allylation of Chiral β‐Stereogenic Alcohols: Bypassing Discrete Formation of Epimerizable Aldehydes. , 2013 .

[39]  M. Krische,et al.  Protecting-group-free diastereoselective C-C coupling of 1,3-glycols and allyl acetate through site-selective primary alcohol dehydrogenation. , 2013, Angewandte Chemie.

[40]  M. Krische,et al.  Enantioselective Carbonyl Allylation and Crotylation from the Alcohol Oxidation Level via C–C Bond Forming Transfer Hydrogenation , 2013 .

[41]  M. Krische,et al.  Site-Selective Primary Alcohol Dehydrogenation Enables Protecting Group-Free Diastereoselective C-C Coupling of 1,3- Glycols and Allyl Acetate** , 2013 .

[42]  Joyce C. Leung,et al.  Ruthenium-catalyzed reductive coupling of 1,3-enynes and aldehydes by transfer hydrogenation: anti-diastereoselective carbonyl propargylation. , 2012, Chemistry.

[43]  M. Krische,et al.  Chiral-anion-dependent inversion of diastereo- and enantioselectivity in carbonyl crotylation via ruthenium-catalyzed butadiene hydrohydroxyalkylation. , 2012, Journal of the American Chemical Society.

[44]  M. Krische,et al.  Iridium-catalyzed allylation of chiral β-stereogenic alcohols: bypassing discrete formation of epimerizable aldehydes. , 2012, Organic letters.

[45]  M. Krische,et al.  Enantioselective carbonyl propargylation by iridium-catalyzed transfer hydrogenative coupling of alcohols and propargyl chlorides. , 2012, Angewandte Chemie.

[46]  M. Krische,et al.  Enantioselective conversion of primary alcohols to α-exo-methylene γ-butyrolactones via iridium-catalyzed C-C bond-forming transfer hydrogenation: 2-(alkoxycarbonyl)allylation. , 2012, Journal of the American Chemical Society.

[47]  M. Krische,et al.  Enantioselective C-H Crotylation of Primary Alcohols via Hydrohydroxyalkylation of Butadiene , 2012, Science.

[48]  M. Krische,et al.  Consecutive iridium catalyzed C-C and C-H bond forming hydrogenations for the diastereo- and enantioselective synthesis of syn-3-fluoro-1-alcohols: C-H (2-fluoro)allylation of primary alcohols. , 2012, Chemical communications.

[49]  Joyce C. Leung,et al.  Diastereo- and enantioselective iridium-catalyzed carbonyl propargylation from the alcohol or aldehyde oxidation level: 1,3-enynes as allenylmetal equivalents. , 2012, Angewandte Chemie.

[50]  M. Krische,et al.  Formation of C–C bonds via ruthenium-catalyzed transfer hydrogenation , 2012, Pure and applied chemistry. Chimie pure et appliquee.

[51]  M. Yus,et al.  Catalytic Enantioselective Allylation of Carbonyl Compounds and Imines , 2012 .

[52]  M. Krische,et al.  Formation of C-C Bonds via Iridium-Catalyzed Hydrogenation and Transfer Hydrogenation. , 2011, Topics in organometallic chemistry.

[53]  M. Krische,et al.  Unlocking Hydrogenation for C-C Bond Formation: A Brief Overview of Enantioselective Methods. , 2011, Organic process research & development.

[54]  M. Krische,et al.  Polarity inversion of donor-acceptor cyclopropanes: disubstituted δ-lactones via enantioselective iridium catalysis. , 2011, Journal of the American Chemical Society.

[55]  Y. Tu,et al.  Direct Sp3 α‐C—H Activation and Functionalization of Alcohol and Ether , 2011 .

[56]  M. Krische,et al.  Catalytic enantioselective Grignard Nozaki-Hiyama methallylation from the alcohol oxidation level: chloride compensates for π-complex instability. , 2011, Chemical communications.

[57]  Yinsheng Zhang,et al.  Use of an Iridium-Catalyzed Redox-Neutral Alcohol-Amine Coupling on Kilogram Scale for the Synthesis of a GlyT1 Inhibitor , 2011 .

[58]  M. Krische,et al.  Direct generation of acyclic polypropionate stereopolyads via double diastereo- and enantioselective iridium-catalyzed crotylation of 1,3-diols: beyond stepwise carbonyl addition in polyketide construction. , 2011, Journal of the American Chemical Society.

[59]  M. Krische,et al.  Diastereo- and enantioselective ruthenium-catalyzed hydrohydroxyalkylation of 2-silyl-butadienes: carbonyl syn-crotylation from the alcohol oxidation level. , 2011, Journal of the American Chemical Society.

[60]  M. Krische,et al.  Iridium-catalyzed anti-diastereo- and enantioselective carbonyl (α-trifluoromethyl)allylation from the alcohol or aldehyde oxidation level. , 2011, Angewandte Chemie.

[61]  M. Krische,et al.  Enantioselective iridium-catalyzed vinylogous Reformatsky-aldol reaction from the alcohol oxidation level: linear regioselectivity by way of carbon-bound enolates. , 2011, Angewandte Chemie.

[62]  Y. Tu,et al.  Direct Sp3α-C-H activation and functionalization of alcohol and ether. , 2011, Chemical Society reviews.

[63]  Takeyuki Suzuki Organic synthesis involving iridium-catalyzed oxidation. , 2011, Chemical reviews.

[64]  M. Krische,et al.  Enhanced anti-diastereo- and enantioselectivity in alcohol-mediated carbonyl crotylation using an isolable single component iridium catalyst. , 2011, The Journal of organic chemistry.

[65]  X. Hou,et al.  Catalytic asymmetric propargylation. , 2011, Chemical reviews.

[66]  M. Krische,et al.  Iridium-catalyzed anti-diastereo- and enantioselective carbonyl (trimethylsilyl)allylation from the alcohol or aldehyde oxidation level. , 2010, Journal of the American Chemical Society.

[67]  M. Krische,et al.  anti-Diastereo- and enantioselective carbonyl (hydroxymethyl)allylation from the alcohol or aldehyde oxidation level: allyl carbonates as allylmetal surrogates. , 2010, Journal of the American Chemical Society.

[68]  M. Krische,et al.  Enantioselective Iridium‐Catalyzed Carbonyl Allylation from the Alcohol Oxidation Level via Transfer Hydrogenation: Minimizing Pre‐Activation for Synthetic Efficiency , 2010 .

[69]  M. Yus,et al.  Hydrogen autotransfer in the N-alkylation of amines and related compounds using alcohols and amines as electrophiles. , 2010, Chemical reviews.

[70]  M. Krische,et al.  Enantioselective carbonyl allylation, crotylation, and tert-prenylation of furan methanols and furfurals via iridium-catalyzed transfer hydrogenation. , 2010, The Journal of organic chemistry.

[71]  R. Crabtree,et al.  Dehydrogenation as a substrate-activating strategy in homogeneous transition-metal catalysis. , 2010, Chemical reviews.

[72]  M. Krische,et al.  Diastereo- and enantioselective anti-alkoxyallylation employing allylic gem-dicarboxylates as allyl donors via iridium-catalyzed transfer hydrogenation. , 2010, Journal of the American Chemical Society.

[73]  M. Krische,et al.  Enantioselective iridium-catalyzed carbonyl allylation from the alcohol oxidation level via transfer hydrogenation: minimizing pre-activation for synthetic efficiency. , 2009, Chemical communications.

[74]  M. Krische,et al.  anti-Diastereo- and Enantioselective Carbonyl Crotylation from the Alcohol or Aldehyde Oxidation Level Employing a Cyclometalated Iridium Catalyst: α-Methyl Allyl Acetate as a Surrogate to Preformed Crotylmetal Reagents. , 2009 .

[75]  M. Krische,et al.  Direct Vinylation of Alcohols or Aldehydes Employing Alkynes as Vinyl Donors: A Ruthenium-Catalyzed C—C Bond-Forming Transfer Hydrogenation. , 2009 .

[76]  M. Krische,et al.  Elongation of 1,3-polyols via iterative catalyst-directed carbonyl allylation from the alcohol oxidation level. , 2009, Organic letters.

[77]  M. Krische,et al.  1,n-glycols as dialdehyde equivalents in iridium-catalyzed enantioselective carbonyl allylation and iterative two-directional assembly of 1,3-polyols. , 2009, Angewandte Chemie.

[78]  M. Krische,et al.  Enantioselective carbonyl reverse prenylation from the alcohol or aldehyde oxidation level employing 1,1-dimethylallene as the prenyl donor. , 2009, Journal of the American Chemical Society.

[79]  D. Hall,et al.  Allylboration of Carbonyl Compounds , 2009 .

[80]  R. W. Hoffmann,et al.  Redox economy in organic synthesis. , 2009, Angewandte Chemie.

[81]  M. Krische,et al.  anti-Diastereo- and enantioselective carbonyl crotylation from the alcohol or aldehyde oxidation level employing a cyclometallated iridium catalyst: alpha-methyl allyl acetate as a surrogate to preformed crotylmetal reagents. , 2009, Journal of the American Chemical Society.

[82]  M. Krische,et al.  Direct vinylation of alcohols or aldehydes employing alkynes as vinyl donors: a ruthenium catalyzed C-C bond-forming transfer hydrogenation. , 2009, Journal of the American Chemical Society.

[83]  M. Whittlesey,et al.  Transition metal catalysed reactions of alcohols using borrowing hydrogen methodology. , 2009, Dalton transactions.

[84]  Michael J. Krische,et al.  Enantioselective iridium-catalyzed carbonyl allylation from the alcohol or aldehyde oxidation level via transfer hydrogenative coupling of allyl acetate: departure from chirally modified allyl metal reagents in carbonyl addition. , 2008, Journal of the American Chemical Society.

[85]  M. Krische,et al.  Ruthenium-catalyzed C-C bond forming transfer hydrogenation: carbonyl allylation from the alcohol or aldehyde oxidation level employing acyclic 1,3-dienes as surrogates to preformed allyl metal reagents. , 2008, Journal of the American Chemical Society.

[86]  M. Krische,et al.  Carbonyl propargylation from the alcohol or aldehyde oxidation level employing 1,3-enynes as surrogates to preformed allenylmetal reagents: a ruthenium-catalyzed C-C bond-forming transfer hydrogenation. , 2008, Angewandte Chemie.

[87]  M. Krische,et al.  Enantioselective iridium-catalyzed carbonyl allylation from the alcohol or aldehyde oxidation level using allyl acetate as an allyl metal surrogate. , 2008, Journal of the American Chemical Society.

[88]  M. Krische,et al.  Catalytic C-C coupling via transfer hydrogenation: reverse prenylation, crotylation, and allylation from the alcohol or aldehyde oxidation level. , 2007, Journal of the American Chemical Society.

[89]  P. Guiry,et al.  The Development of the Asymmetric Nozaki–Hiyama–Kishi Reaction , 2007 .

[90]  I. Marek,et al.  Creation of Quaternary Stereocenters in Carbonyl Allylation Reactions , 2007 .

[91]  Jonathan M. J. Williams,et al.  Borrowing hydrogen in the activation of alcohols , 2007 .

[92]  D. Hall Lewis and Brønsted Acid Catalyzed Allylboration of Carbonyl Compounds: From Discovery to Mechanism and Applications , 2007 .

[93]  M. Yus,et al.  Alcohols as electrophiles in C--C bond-forming reactions: the hydrogen autotransfer process. , 2007, Angewandte Chemie.

[94]  D. Ripin,et al.  Large‐Scale Oxidations in the Pharmaceutical Industry , 2006 .

[95]  Chan-Mo Yu,et al.  Regulation of Stereoselectivity and Reactivity in the Inter‐ and Intramolecular Allylic Transfer Reactions , 2006 .

[96]  J. S. Carey,et al.  Analysis of the reactions used for the preparation of drug candidate molecules. , 2006, Organic & biomolecular chemistry.

[97]  D. Ripin,et al.  Survey of GMP Bulk Reactions Run in a Research Facility between 1985 and 2002 , 2005 .

[98]  B. W. Gung Additions of Allyl, Allenyl, and Propargylstannanes to Aldehydes and Imines , 2004 .

[99]  S. Denmark,et al.  Catalytic Enantioselective Addition of Allylic Organometallic Reagents to Aldehydes and Ketones , 2003 .

[100]  P. Ramachandran Pinane‐Based Versatile “Allyl” Boranes , 2003 .

[101]  P. Verhoest,et al.  Total synthesis of (+)-phorboxazole A exploiting the Petasis-Ferrier rearrangement. , 2001, Journal of the American Chemical Society.

[102]  B. Heller,et al.  How Long Have Nonlinear Effects Been Known in the Field of Catalysis , 2000 .

[103]  B. Bartels,et al.  Ir‐Catalyzed Allylic Substitution: Mechanistic Aspects and Asymmetric Synthesis with Phosphorus Amidites as Ligands. , 1999 .

[104]  G. Helmchen,et al.  Ir-catalysed allylic substitution: mechanistic aspects and asymmetric synthesis with phosphorus amidites as ligands , 1999 .

[105]  M. Kashio,et al.  Iridium Complex-Catalyzed Allylic Alkylation of Allylic Esters and Allylic Alcohols: Unique Regio- and Stereoselectivity , 1998 .

[106]  G. Helmchen,et al.  First Enantioselective Alkylations of Monosubstituted Allylic Acetates Catalyzed by Chiral Iridium Complexes , 1997 .

[107]  K. Rossen,et al.  A New Planar Chiral Bisphosphine Ligand for Asymmetric Catalysis: Highly Enantioselective Hydrogenations under Mild Conditions. , 1997 .

[108]  R. Takeuchi,et al.  Highly Selective Allylic Alkylation with a Carbon Nucleophile at the More Substituted Allylic Terminus Catalyzed by an Iridium Complex: An Efficient Method for Constructing Quaternary Carbon Centers. , 1997 .

[109]  J. A. Marshall Chiral Allylic and Allenic Stannanes as Reagents for Asymmetric Synthesis. , 1996, Chemical reviews.

[110]  R. W. Hoffmann,et al.  Enantioselective Synthesis of Homoallyl Alcohols via Chiral Allylboronic Esters , 1978 .

[111]  Jean-Pierre Vigneron,et al.  Nouvelle methode pour porter au maximum la purete optique d'un produit partiellement dedouble sans l'aide d'aucune substance chirale , 1973 .