Recent Publications

Undergraduate Laboratory Manual

Working with Dr. Cynthia McGowan (Merrimack College MA) we have published a laboratory manual focused on microwave-promoted synthesis for use in the undergraduate organic teaching laboratory. By integrating microwave-promoted chemistry into undergraduate laboratory courses it is possible not only to train students in using a new technique but also to widen the scope of the reactions that they can perform. Since reaction times are so much shorter than when using conventional heating, students can be introduced to chemistry that would have otherwise been inaccessible because the experiment took too long for a lab period (for example, involving an overnight reflux). Also, microwave heating gives students the ability to repeat an experiment within the same laboratory period if they need to. Many of the reactions presented in the book are performed either solvent-free or else using water as solvent. This makes them clean as well as efficient and allow for introduction of the concepts of “green chemistry”. All of the reactions have been trialed on groups of students in our laboratory classes before being selected for the book. The book comprises of two introductory chapters followed by procedures for eleven different reactions. Two procedures for each experiment are given, one for use with a single-vessel microwave unit and one for use with a microwave that can hold up to 40 vessels. This means that smaller and larger student groups can use the manual.

Below is a list of our recent publications (2000-present).
If you would like an electronic reprint of any of them, do not hesitate to contact Dr. Leadbeater.

Shoemaker, K.A., Leadbeater, N.E. A fast and easy approach to the synthesis of Zeise’s salt using microwave heating, Inorganic Chemistry Communications, 2009, 12, 341-342.

Schmink, J.R.; Leadbeater, N.E. Palladium-Catalyzed Synthesis of Diarylmethanes: Exploitation of Carbanionic Leaving Groups, Organic Letters, 2009, 11 (12), 2575-2578.

Stencel, L.M.; Kormos, C.M.; Avery, K.B.; Leadbeater, N.E. Assessment and use of two silicon carbide multi-well plates for library synthesis and proteolytic digests using microwave heating, Organic & Biomolecular Chemistry, 2009, 7, 2452-2457.

Avery, K.B.; Devine, W.G.; Kormos, C.M.; Leadbeater, N.E. Use of a silicon carbide multi-well plate in conjunction with microwave heating for rapid ligand synthesis, formation of palladium complexes and catalyst screening in a Suzuki coupling, Tetrahedron Letters, 2009, 50 (24), 2851-2853.

Iannelli, M.; Bergamelli, F.; Kormos, C.M.; Paravisi, S; Leadbeater, N.E. Application of a batch microwave unit for scale-up of alkoxycarbonylation reactions using a near-stoichiometric loading of carbon monoxide, Organic Process Research & Development, 2009, 13 (3), 634-637.

Kormos, C.M; Hull, R.M.; Leadbeater, N.E. Microwave Heating in Conjunction with UV Irradiation: a Tool for the Oxidation of 1,4-Dihydropyridines to Pyridines, Australian Journal of Chemistry, 2009, 62, 51-57.

Schmink, J.R.; Holcomb, J.L.; Leadbeater, N.E. Testing the Validity of Microwave-Interfaced, in Situ Raman Spectroscopy as a Tool for Kinetic Studies, Organic Letters, 2009, 11 (2), 365-368.

McGowan, C. M.; Leadbeater, N. E. Clean, Fast Palladium-Catalyzed Reactions using Microwave Heating and Water as a solvent: The Heck Coupling as an Example, in Experiments in Green and Sustainable Chemistry, Roesky, H. W.; Kennepohl, D. K. Eds, Wiley-VCH, Weinheim, 2009, 97-107.

Voutchkova, A. Coplin, A.; Leadbeater, N. E.; Crabtree. R. H. Palladium-Catalyzed Decarboxylative Coupling of Aromatic Acids with Aryl Halides or Unactivated Arenes Using Microwave Heating, Chemical Communications, 2008, 6312-6314.

Schmink, J.R., Holcomb, J.L.; Leadbeater, N.E. Use of Raman spectroscopy as an In Situ Tool to Obtain Kinetic Data for Organic Transformations, Chemistry: A European Journal, 2008, 14, 9943-9950.

Bowman, M. D.; Schmink, J. R.; McGowan, C. M.; Kormos, C. M.; Leadbeater, N. E. Scale-Up of Microwave-Promoted Reactions to the Multigram Level Using a Sealed-Vessel Microwave Apparatus, Organic Process Research & Development, 2008, 12 (6), 1078-1088.

Velmathi, S.; Leadbeater, N. E.; Palladium-catalyzed cyanation of aryl halides using K₄[Fe(CN)₆] as cyanide source, water as solvent, and microwave heating, Tetrahedron Letters, 2008, 49 (32), 4693-4694.

Kormos, C. M.; Leadbeater, N. E. Preparation of Nonsymmetrically Substituted Stilbenes in a One-Pot Two-Step Heck Strategy Using Ethene As a Reagent, Journal of Organic Chemistry, 2008, 73, 3854-3858.

Leadbeater, N. E.; Shoemaker, K. M. Preparation of Ruthenium and Osmium Carbonyl Complexes Using Microwave Heating: Demonstrating the Use of a Gas-Loading Accessory and Real-Time Reaction Monitoring by Means of a Digital Camera, Organometallics, 2008, 27 (6), 1254-1258.

Bowman, M. D.; Holcomb, J. L.; Kormos, C. M.; Leadbeater, N. E.; Williams, V. A. Approaches for Scale-Up of Microwave-Promoted Reactions, Organic Process Research and Development, 2008, 12, 41-57.

Bowman, M. D.; Leadbeater, N. E.; Barnard, T. M. Watching microwave-promoted chemistry: reaction monitoring using a digital camera interfaced with a scientific microwave apparatus, Tetrahedron Letters, 2008, 49, 195-198.

Dean, M. L.; Schmink, J. R.; Leadbeater, N. E.; Brückner, C. Microwave-promoted insertion of Group 10 metals into free base porphyrins and chlorins: scope and limitations. Dalton Transactions, 2008, 1341-1345.

Leadbeater, N. E.; Schmink, J. R. Use of Raman spectroscopy as a tool for in situ monitoring of microwave-promoted reactions, Nature Protocols, 2008, 3, 1-7.

Leadbeater, N. E.; Khan, M. R. Microwave-Promoted Desulfurization of Heavy and Sulfur-Containing Crude Oil, Energy and Fuels, 2008, 22 (3), 1836-1839.

Leadbeater, N. E.; Barnard, T. M.; Stencel, L. M. Batch and continuous-flow preparation of biodiesel derived from vegetable oil and butanol using acid catalysis facilitated by microwave heating, Energy and Fuels, 2008, 22 (3), 2005-2008.

Leadbeater, N. E.; Smith, R. J. In situ Raman spectroscopy as a probe for the effect of power on microwave-promoted Suzuki coupling reactions. Organic & Biomolecular Chemistry, 2007, 5 (17), 2770-2774.

Kormos, C. M.; Leadbeater, N. E. Alkoxycarbonylation reactions performed using near stoichiometric quantities of CO, Synlett, 2007, 2006-2010.

Barnard, T. M.; Leadbeater, N. E.; Boucher, M. B.; Stencel, L. M.; Wilhite, B. A. Continuous-Flow Preparation of Biodiesel Using Microwave Heating, Energy and Fuels, 2007, 1777.

Collins, J. M.; Leadbeater, N. E. Microwave energy: a versatile tool for the biosciences, Organic & Biomolecular Chemistry, 2007, 1141-1150.

Amore, K. M.; Leadbeater, N. E. Microwave-Promoted Esterification Reactions: Optimization and Scale-Up, Macromolecular Rapid Communications, 2007, 28, 473-477.

Leadbeater, N. E.; Smith, R. J.; Barnard, T. M. Using in situ Raman monitoring as a tool for rapid optimisation and scale-up of microwave-promoted organic synthesis: esterification as an example, Organic & Biomolecular Chemistry, 2007, 822-825.

Leadbeater, N. E.; Stencel, L. M.; Wood, E. C. Probing the effects of microwave irradiation on enzyme-catalysed organic transformations: the case of lipase-catalysed transesterification reactions, Organic & Biomolecular Chemistry, 2007, 1052-1055.

Leadbeater, N. E.; Schmink, J.R. Use of a scientific microwave apparatus for rapid optimization of reaction conditions in a monomode function and then substrate screening in a multimode function, Tetrahedron, 2007, 63, 6764-6773.

Amore, K. M.; Leadbeater, N. E.; Miller, T. A.; Schmink, J. R. Fast, easy, solvent-free, microwave-promoted Michael addition of anilines to α,β-unsaturated alkenes: synthesis of N-aryl functionalized β-amino esters and acids, Tetrahedron Letters, 2006, 47, 8583-8586.

Kormos, C. M.; Leadbeater N. E. Alkoxycarbonylation of aryl iodides using gaseous carbon monoxide and pre-pressurized reaction vessels in conjunction with microwave heating, Organic & Biomolecular Chemistry, 2007, 65-68.

Leadbeater, N. E.; Smith, R. J. Real-Time Monitoring of Microwave-Promoted Suzuki Coupling Reactions Using in Situ Raman Spectroscopy, Organic Letters, 2006, 8 (20), 4589-4591.

Leadbeater, N. E.; Williams, V. A., Barnard, T. M.; Collins, M. J. Solvent-free, open-vessel microwave-promoted Heck couplings: From the mmol to the mol scale, Synlett, 2006, 2953-2958.

Barnard, T. M.; Leadbeater, N. E. Real-time monitoring of microwave-promoted organometallic ligand-substitution reactions using in-situ Raman spectroscopy, Chemical Communications, 2006, 3615-3616.

Leadbeater, N. E.; Stencel, L. M. Fast, easy preparation of biodiesel using microwave heating, Energy and Fuels, 2006, 20, 2281-2283.

Kormos, C. M.; Leadbeater N. E. Microwave-Promoted Hydroxycarbonylation in Water Using Gaseous Carbon Monoxide and Pre-Pressurized Reaction Vessels, Synlett, 2006, 1663-1666.

Leadbeater, N. E.; Williams, V. A.; Barnard T. M.; Collins M. J. Open-Vessel Microwave-Promoted Suzuki Reactions Using Low Levels of Palladium Catalyst: Optimization and Scale-Up, Organic Process Research and Development, 2006, 10, 833-837.

Leadbeater, N. E. Microwaves in organic chemistry – Preface to a Symposium in Print, Tetrahedron, 2006, 62, 4633.

Kormos, C. M.; Leadbeater, N. E. Direct conversion of aryl halides to phenols using high temperature or near-critical water and microwave heating, Tetrahedron, 2006, 62, 4728-4732.

Chanthavong, F.; Leadbeater, N. E. The application of organic bases in microwave-promoted Suzuki coupling reactions in water, Tetrahedron Letters, 2006, 47, 1909-1912.

Arvela, R. K.; Leadbeater, N. E.; Mack, T. L.; Kormos, C. M. Microwave-promoted Suzuki coupling reactions with organotrifluoroborates in water using ultra-low catalyst loadings, Tetrahedron Letters, 2006, 47, 217-220.

Arvela, R. K.; Leadbeater, N. E.; Collins, M. J. Automated batch scale-up of microwave-promoted Suzuki and Heck coupling reactions in water using ultra-low metal catalyst concentrations, Tetrahedron, 2005, 61, 9349-9355.

Leadbeater, N. E. Fast, easy, clean chemistry by using water as a solvent and microwave heating: the Suzuki coupling as an illustration, Chemical Communications, 2005, 2881-2902.

Arvela, R. K.; Leadbeater, N. E. Suzuki coupling of aryl chlorides with phenylboronic acid in water, using microwave heating with simultaneous cooling, Organic Letters, 2005, 7, 2101-2104.

Leadbeater, N. E.; Pillsbury, S. J.; Shanahan, E.; Williams V. A. An assessment of the technique of simultaneous cooling in conjunction with microwave heating for organic synthesis, Tetrahedron, 2005, 61, 3565-3585.

Arvela, R. K.; Leadbeater, N. E. Microwave-promoted Heck coupling using ultralow metal catalyst concentrations, Journal of Organic Chemistry, 2005, 70, 1786-1790.

Arvela, R. K.; Leadbeater, N. E.; Sangi, M. S.; Williams, V. A.; Granados, P.; Singer, R. D. A reassessment of the transition-metal free Suzuki-type coupling methodology, Journal of Organic Chemistry, 2005, 70, 161-168.

Leadbeater, N. E.; Torenius, H. M.; Tye, H. Microwave-promoted organic synthesis using ionic liquids: A mini review, Combinatorial Chemistry and High Throughput Screening, 2004, 7, 511-528.

Leadbeater, N. E. Ionic liquids and their heating behaviour during microwave irradiation - a state of the art report and challenge to assessment, Green Chemistry, 2003, 5, 677-678.

Leadbeater, N. E.; Tominack, B. J. Rapid, easy copper-free Sonogashira couplings using aryl iodides and activated aryl bromides, Tetrahedron Letters, 2003, 44, 8653-8656.

Leadbeater, N.E. Microwaves in organic chemistry, Tetrahedron, 2003, 4633.

Arvela, R. K.; Leadbeater, N. E. Rapid, easy cyanation of aryl bromides and chlorides using nickel salts in conjunction with microwave promotion, Journal of Organic Chemistry, 2003, 68, 9122-9125.

Leadbeater, N. E.; Marco, M.; Tominack, B. J. First examples of transition-metal free Sonogashira-type couplings, Organic Letters, 2003, 5, 3919-3922.

Leadbeater, N. E.; Sharp, E. L. Preparation of resin-bound metal carbonyl reagents and preliminary demonstration of their use, Organometallics, 2003, 22, 4167-4169.

Leadbeater, N. E.; Marco, M. Transition-metal-free Suzuki-type coupling reactions: Scope and limitations of the methodology, Journal of Organic Chemistry, 2003, 68, 5660-5667.

Arvela, R. K.; Leadbeater, N. E. Fast and easy halide exchange in aryl halides, Synlett, 2003, 1145-1148.

Leadbeater, N. E.; Marco, M. Transition-metal-free Suzuki-type coupling reactions, Angewandte Chemie International Edition, 2003, 42, 1407-1409.

Arvela, R. K.; Leadbeater, N. E.; Torenius, H. M.; Tye. H. Rapid cyanation of aryl iodides in water using microwave promotion, Organic and Biomolecular Chemistry, 2003, 1, 1119-1121.

Leadbeater, N. E.; Torenius, H. M.; Tye, H. Ionic liquids as reagents and solvents in conjunction with microwave heating: rapid synthesis of alkyl halides from alcohols and nitriles from aryl halides, Tetrahedron, 2003, 59, 2253-2258.

Leadbeater, N. E.; Marco. M. Rapid and amenable Suzuki coupling reaction in water using microwave and conventional heating, Journal of Organic Chemistry, 2003, 68, 888-892.

Klingensmith, L. M.; Leadbeater, N. E. Ligand-free palladium catalysis of aryl coupling reactions facilitated by grinding, Tetrahedron Letters, 2003, 44, 765-768.

Leadbeater, N. E. Polymer-supported metal-phosphine complexes for use as catalysts or linkers in medicinally-oriented organic synthesis, Current Medicinal Chemistry, 2002, 9, 2147-2171.

Leadbeater, N. E.; Marco, M. Preparation of polymer-supported ligands and metal complexes for use in catalysis, Chemical Reviews, 2002, 102, 3217-3274.

Grainger, R. S.; Leadbeater, N. E.; Pamies, A. M. The tetramethylguanidine catalyzed Baylis-Hillman reaction: Effects of co-catalysts and alcohol solvents on reaction rate, Catalysis Communications, 2002, 3, 449-452.

Leadbeater, N. E.; Marco, M. Ligand-free palladium catalysis of the Suzuki reaction in water using microwave heating, Organic Letters, 2002, 4, 2973-2976.

Bräse, S.; Dahmen S.; Lauterwasser F.; Leadbeater, N. E.; Sharp, E. L. Polymer-bound 1-aryl-3-alkyltriazenes as modular ligands for catalysis. Part 1: Synthesis and metal coordination, Bioorganic and Medicinal Chemistry Letters, 2002, 12, 1845-1848.

Bräse, S.; Dahmen S.; Lauterwasser F.; Leadbeater, N. E.; Sharp, E. L. Polymer-bound 1-aryl-3-alkyltriazenes as modular ligands for catalysis. Part 2: Screening immobilized metal complexes for catalytic activity Bioorganic and Medicinal Chemistry Letters, 2002, 12, 1849-1851.

Lattanzi, A,; Leadbeater, N. E. Microencapsulated VO(acac)(2): Preparation and use in allylic alcohol epoxidation, Organic Letters, 2002, 4, 1519-1521.

Leadbeater, N. E.; Torenius, H. M. A study of the ionic liquid mediated microwave heating of organic solvents, Journal of Organic Chemistry, 2002, 67, 3145-3148.

Leadbeater N. E. Facile synthesis of polymer-supported cyclopentadienes, Tetrahedron Letters, 2002, 43, 691-693.

Leadbeater, N. E.; van der Pol, C. Development of catalysts for the Baylis-Hillman reaction: the application of tetramethylguanidine and attempts to use a supported analogue, Journal of the Chemical Society – Perkin Transactions 1, 2001, 2831-2835.

Leadbeater,N. E. Bis-cyclopentadienyl nickel (nickelocene): A convenient starting material for reactions catalyzed by Ni(0) phosphine complexes, Journal of Organic Chemistry, 2001, 66, 7539-7541.

Leadbeater, N. E.; van der Pol, C. Preparation of resin-bound amine N-oxides and demonstration of their use in synthetic carbonyl cluster chemistry, Chemical Communications, 2001, 599-600.

Leadbeater N. E. Preparation of a resin-bound ruthenium phosphine complex and assessment of its use in transfer hydrogenation and hydrocarbon oxidation, Journal of Organic Chemistry, 2001, 66, 2168-2170.

Leadbeater, N. E.; Scott, K. A. Preparation of a resin-bound cobalt phosphine complex and assessment of its use in catalytic oxidation and acid anhydride synthesis, Journal of Organic Chemistry, 2000, 65, 4770-4772.

Leadbeater N. E.; Scott, K. A.; Scott, L. J. Preparation of a resin-bound arene-ruthenium complex and assessment of its use in enol formate synthesis and olefin cyclopropanation, Journal of Organic Chemistry, 2000, 65, 3231-3232.

Griffiths C.; Leadbeater, N. E. Palladium and nickel catalysed Suzuki cross-coupling of sterically hindered aryl bromides with phenylboronic acid, Tetrahedron Letters, 2000, 41, 2487-2490.