Practical, Broadly Applicable, α-Selective, Z-Selective, Diastereoselective, and Enantioselective Addition of Allylboron Compounds to Mono-, Di-, Tri-, and Polyfluoroalkyl Ketones.

A practical method for enantioselective synthesis of fluoroalkyl-substituted Z-homoallylic tertiary alcohols has been developed. Reactions may be performed with ketones containing a polylfluoro-, trifluoro-, difluoro-, and monofluoroalkyl group along with an aryl, a heteroaryl, an alkenyl, an alkynyl, or an alkyl substituent. Readily accessible unsaturated organoboron compounds serve as reagents. Transformations were performed with 0.5-2.5 mol % of a boron-based catalyst, generated in situ from a readily accessible valine-derived aminophenol and a Z- or an E-γ-substituted boronic acid pinacol ester. With a Z organoboron reagent, additions to trifluoromethyl and polyfluoroalkyl ketones proceeded in 80-98% yield, 97:3 to >98:2 α:γ selectivity, >95:5 Z:E selectivity, and 81:19 to >99:1 enantiomeric ratio. In notable contrast to reactions with unsubstituted allylboronic acid pinacol ester, additions to ketones with a mono- or a difluoromethyl group were highly enantioselective as well. Transformations were similarly efficient and α- and Z-selective when an E-allylboronate compound was used, but enantioselectivities were lower. In certain cases, the opposite enantiomer was favored (up to 4:96 er). With a racemic allylboronate reagent that contains an allylic stereogenic center, additions were exceptionally α-selective, affording products expected from γ-addition of a crotylboron compound, in up to 97% yield, 88:12 diastereomeric ratio, and 94:6 enantiomeric ratio. Utility is highlighted by gram-scale preparation of representative products through transformations that were performed without exclusion of air or moisture and through applications in stereoselective olefin metathesis where Z-alkene substrates are required. Mechanistic investigations aided by computational (DFT) studies and offer insight into different selectivity profiles.

[1]  Malte S. Mikus,et al.  Electronically Activated Organoboron Catalysts for Enantioselective Propargyl Addition to Trifluoromethyl Ketones. , 2017, Angewandte Chemie.

[2]  E. Meggers,et al.  Octahedral Ruthenium Complex with Exclusive Metal-Centered Chirality for Highly Effective Asymmetric Catalysis. , 2017, Journal of the American Chemical Society.

[3]  N. Kumagai,et al.  Catalytic asymmetric synthesis of CF3-substituted tertiary propargylic alcohols via direct aldol reaction of α-N3 amide , 2017, Chemical science.

[4]  R. Schrock,et al.  Molybdenum chloride catalysts for Z-selective olefin metathesis reactions , 2017, Nature.

[5]  K. Szabó,et al.  Recent Advances in the Preparation and Application of Allylboron Species in Organic Synthesis. , 2017, Journal of the American Chemical Society.

[6]  A. Hoveyda,et al.  Practical and Broadly Applicable Catalytic Enantioselective Additions of Allyl-B(pin) Compounds to Ketones and α-Ketoesters. , 2016, Angewandte Chemie.

[7]  J. Morken,et al.  Modular, Catalytic Enantioselective Construction of Quaternary Carbon Stereocenters by Sequential Cross-Coupling Reactions. , 2016, Organic letters.

[8]  A. Hoveyda,et al.  Catalytic enantioselective addition of organoboron reagents to fluoroketones controlled by electrostatic interactions , 2016, Nature Chemistry.

[9]  A. Hoveyda,et al.  Lewis Acid Catalyzed Borotropic Shifts in the Design of Diastereo- and Enantioselective γ-Additions of Allylboron Moieties to Aldimines. , 2016, Angewandte Chemie.

[10]  C. Wolf,et al.  Efficient Access to Multifunctional Trifluoromethyl Alcohols through Base-Free Catalytic Asymmetric C-C Bond Formation with Terminal Ynamides. , 2016, Angewandte Chemie.

[11]  R. Schrock,et al.  Direct synthesis of Z-alkenyl halides through catalytic cross-metathesis , 2016, Nature.

[12]  C. Schofield,et al.  Cation–π Interactions Contribute to Substrate Recognition in γ‐Butyrobetaine Hydroxylase Catalysis , 2015, Chemistry.

[13]  M. D. Hill,et al.  Applications of Fluorine in Medicinal Chemistry. , 2015, Journal of medicinal chemistry.

[14]  C. Mück‐Lichtenfeld,et al.  Cation-π interactions in iminium ion activation: correlating quadrupole moment & enantioselectivity. , 2015, Chemical communications.

[15]  Malte S. Mikus,et al.  High-value alcohols and higher-oxidation-state compounds by catalytic Z-selective cross-metathesis , 2015, Nature.

[16]  D. O'Hagan,et al.  Successful fluorine-containing herbicide agrochemicals , 2014 .

[17]  A. Sakakura,et al.  Enantioselective 1,3-dipolar cycloaddition of azomethine imines with propioloylpyrazoles induced by chiral π-cation catalysts. , 2014, Journal of the American Chemical Society.

[18]  A. Hoveyda,et al.  An Efficient, Practical, and Enantioselective Method for Synthesis of Homoallenylamides Catalyzed by an Aminoalcohol-Derived, Boron-Based Catalyst , 2014, Journal of the American Chemical Society.

[19]  M. Yus,et al.  Diastereoselective allylation of carbonyl compounds and imines: application to the synthesis of natural products. , 2013, Chemical reviews.

[20]  Jinhua J. Song,et al.  Asymmetric methallylation of ketones catalyzed by a highly active organocatalyst 3,3'-F2-BINOL. , 2013, Organic letters.

[21]  G. N. Sastry,et al.  Cation-π interaction: its role and relevance in chemistry, biology, and material science. , 2013, Chemical reviews.

[22]  M. Snapper,et al.  Simple Organic Molecules as Catalysts for Enantioselective Synthesis of Amines and Alcohols , 2012, Nature.

[23]  D. T. McQuade,et al.  Iterative asymmetric allylic substitutions: syn- and anti-1,2-diols through catalyst control. , 2012, Angewandte Chemie.

[24]  I. A. Roundtree,et al.  Ni- and Pd-catalyzed synthesis of substituted and functionalized allylic boronates. , 2012, Organic letters.

[25]  S. Yamada,et al.  Nitrogen cation-π interactions in asymmetric organocatalytic synthesis. , 2011, Organic & biomolecular chemistry.

[26]  M. Yus,et al.  Catalytic enantioselective allylation of carbonyl compounds and imines. , 2011, Chemical reviews.

[27]  P. Metrangolo,et al.  Organic fluorine compounds: a great opportunity for enhanced materials properties. , 2011, Chemical Society reviews.

[28]  Wenqin Zhang,et al.  Catalytic enantioselective alkynylation of trifluoromethyl ketones: pronounced metal fluoride effects and implications of zinc-to-titanium transmetallation. , 2011, Angewandte Chemie.

[29]  Hershel H. Lackey,et al.  Stereoconvergent synthesis of chiral allylboronates from an E/Z mixture of allylic aryl ethers using a 6-NHC-Cu(I) catalyst. , 2011, Journal of the American Chemical Society.

[30]  Hajime Ito,et al.  Direct enantio-convergent transformation of racemic substrates without racemization or symmetrization , 2010, Nature Chemistry.

[31]  A. Hoveyda,et al.  Enantioselective synthesis of allylboronates bearing a tertiary or quaternary B-substituted stereogenic carbon by NHC-Cu-catalyzed substitution reactions. , 2010, Journal of the American Chemical Society.

[32]  M. Kanai,et al.  Identification of modular chiral bisphosphines effective for Cu(i)-catalyzed asymmetric allylation and propargylation of ketones. , 2010, Journal of the American Chemical Society.

[33]  E. Jacobsen,et al.  Enantioselective thiourea-catalyzed cationic polycyclizations. , 2010, Journal of the American Chemical Society.

[34]  R. Ely,et al.  Regio- and stereoselective Ni-catalyzed 1,4-hydroboration of 1,3-dienes: access to stereodefined (Z)-allylboron reagents and derived allylic alcohols. , 2010, Journal of the American Chemical Society.

[35]  K. Matsuura,et al.  Desymmetrization of meso-2-alkene-1,4-diol derivatives through copper(I)-catalyzed asymmetric boryl substitution and stereoselective allylation of aldehydes. , 2010, Angewandte Chemie.

[36]  S. Peng,et al.  A Spirocyclic Chiral Borate for Catalytic Enantioselective Nozaki-Hiyama Allylation of Ketones , 2009 .

[37]  David S. Barnett,et al.  The mechanism and an improved asymmetric allylboration of ketones catalyzed by chiral biphenols. , 2009, Angewandte Chemie.

[38]  Philip Taynton,et al.  Asymmetric indium-mediated Barbier-type allylation reactions with ketones to form homoallylic alcohol products , 2008 .

[39]  K. Matsuura,et al.  Copper-catalyzed enantioselective substitution of allylic carbonates with diboron: an efficient route to optically active alpha-chiral allylboronates. , 2007, Journal of the American Chemical Society.

[40]  S. Yamada Intramolecular cation-pi interaction in organic synthesis. , 2007, Organic & biomolecular chemistry.

[41]  M. Kanai,et al.  Copper(I) alkoxide-catalyzed alkynylation of trifluoromethyl ketones. , 2007, Organic letters.

[42]  Xiaoming Feng,et al.  Enantioselective allylation of ketones catalyzed by N,N'-dioxide and indium(III) complex. , 2007, The Journal of organic chemistry.

[43]  J. Aubé,et al.  Cation-pi control of regiochemistry of intramolecular schmidt reactions en route to bridged bicyclic lactams. , 2007, Journal of the American Chemical Society.

[44]  M. Sigman,et al.  Design and synthesis of modular oxazoline ligands for the enantioselective chromium-catalyzed addition of allyl bromide to ketones. , 2007, Journal of the American Chemical Society.

[45]  S. Schaus,et al.  Asymmetric allylboration of ketones catalyzed by chiral diols. , 2006, Journal of the American Chemical Society.

[46]  T. Frejd,et al.  Enantioselective synthesis of bridgehead hydroxyl bicyclo[2.2.2]octane derivatives via asymmetric allylindation , 2006 .

[47]  Hisashi Yamamoto,et al.  Silver-catalyzed asymmetric Sakurai-Hosomi allylation of ketones. , 2005, Journal of the American Chemical Society.

[48]  P. Walsh,et al.  Catalytic asymmetric allylation of ketones and a tandem asymmetric allylation/diastereoselective epoxidation of cyclic enones. , 2004, Journal of the American Chemical Society.

[49]  M. Kanai,et al.  Catalytic enantioselective allylboration of ketones. , 2004, Journal of the American Chemical Society.

[50]  K. Maruoka,et al.  Catalytic enantioselective allylation of ketones with novel chiral bis-titanium(IV) catalyst. , 2003, Chirality.

[51]  T. Loh,et al.  An enantioselective indium-mediated allylation reaction of aldehydes and ketones in dichloromethane , 1999 .

[52]  D. A. Dougherty,et al.  The Cationminus signpi Interaction. , 1997, Chemical reviews.

[53]  D. A. Dougherty,et al.  Cation-π Interactions in Chemistry and Biology: A New View of Benzene, Phe, Tyr, and Trp , 1996, Science.

[54]  P. Ramachandran,et al.  Selective reductions. 52. Efficient asymmetric reduction of α-acetylenic α′-fluoroalkyl ketones with either B-chlorodiisopinocampheylborane or B-isopinocampheyl-9-borabicyclo[3.3.1]nonane in high enantiomeric purity. The influence of fluoro groups in such reductions , 1994 .

[55]  Davidr . Evans,et al.  Substrate-directable chemical reactions , 1993 .

[56]  V. I. Mstislavsky,et al.  Determination of the activation parameters of permanent allylic rearrangement in allyl- and methallylboranes and in 1,1-bis(dipropylborylmethyl)ethylene by dynamic NMR spectroscopy , 1992 .

[57]  P. Schleyer,et al.  Allylborane and its isomers. An ab initio study of the C3BH7 potential energy surface, the barrier to 1,3-shifts in allylboranes, and nonclassical boracyclobutane, cyclopropylborane, and vinylborane structures , 1991 .

[58]  J. Snyder,et al.  (1,3)-SIGMATROPIC SHIFTS OF ALLYLAMINE AND ALLYLBORANE. FLEXIBLE MODELS FOR POSSIBLE PSEUDOPERICYCLIC REACTIONS , 1981 .

[59]  K. G. Hancock,et al.  Thermally stable ?-methalallylboranes , 1974 .

[60]  J. D. Ḱramer,et al.  Thermal isomerization of but-1-en-3-yl(dimethylamino)ethylborane. Reluctant 1,3-sigmatropic shift of boron in an unusually stable allylborane , 1973 .