1. Author's Information
    Jin-Kyun Lee
    Melville Laboratory for Polymer Synthesis, Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK

    Rachel M. Williamson
    School of Chemistry, Bio21 Institute, University of Melbourne, VIC 3010, Australia

    Andrew B. Holmes
    Melville Laboratory for Polymer Synthesis, Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK

    Edward J. Bush
    Process R&D, AstraZeneca Pharmaceuticals, Silk Road Business Park, Macclesfield, Cheshire SK10 2NA, UK

    Ian F. McConvey
    Process R&D, AstraZeneca Pharmaceuticals, Silk Road Business Park, Macclesfield, Cheshire SK10 2NA, UK

  2. Abstract
    The effects of electronic and steric properties of phosphorus ligands on Heck reactions in supercritical CO2 and non-polar hydrocarbon solvents were studied. In Heck reactions between iodobenzene and butyl acrylate, higher yields were obtained with less electron-rich phosphine ligands. This trend was also observed with the electron-poor triphenyl phosphite. A range of sterically demanding phosphites were then investigated. Biphenyl-containing phosphites 8 and 13 were found to be highly effective. In the Heck reaction between the less-reactive bromobenzene and butyl acrylate, the bulky, electron-rich tri-tert-butylphosphine ligand produced the best yield. These results emphasize the importance of both electronic and steric properties of phosphorus ligands in the Heck reaction in non-polar solvents.
    Keywords
    Heck Reaction, Non-Polar Hydrocarbon Solvents, Supercritical Carbon Dioxide

    ADLID: 50308-v1
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  1. Keywords
    Heck Reaction Non-Polar Hydrocarbon Solvents Supercritical Carbon Dioxide
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