Home

Register

Agenda

Poster Submissions

Venue

Accommodation

Exhibition

Media Partners

Training Course

8:00am 

Registration

Organic Synthesis
Session Chair: C. Oliver Kappe, Director, Christian Doppler Laboratory for Microwave Synthesis, University of Graz 

9:05am

Keynote Address - Direct Alkylation and Arylation of Nitrogen Heterocycles Utilizing Microwave Chemistry
Jonathan Ellman, Professor, University of California - Berkeley
Nitrogen heterocycles are prevalent in drugs, drug candidates and bioactive natural products. Consequently, the metal-catalyzed direct functionalization of nitrogen heterocycles has the potential to greatly impact drug discovery research. In this seminar, rhodium-catalyzed methods will be presented for the microwave-mediated direct alkylation and arylation of nitrogen heterocycles using readily available alkene and aryl halide inputs.

9:50am

Five Years of Microwave-Assisted Carbonylations: Preparative Advances and Lessons Learned
Mats Larhed, Head of Division, Uppsala University
Controlled microwave heating has emerged as an enabling and productivity-enhancing tool for the organic and medicinal chemist. With this superheating method, reaction times can often be reduced from days and hours down to minutes, and chemistry previously considered impractical or unattainable can be accessed. In this presentation, microwave-accelerated carbonylations of aryl halides and triflates will be discussed. Molybdenum hexacarbonyl was used as a solid CO-source, avoiding the risk and troublesome handling associated with the use of CO-gas. Examples were chosen to illustrate the large diversity of microwave methods within this class of palladium(0)-catalyzed reactions, including the use of new nucleophiles, applications in medicinal chemistry and reactions performed in neat water. In most cases, reactions were performed in small scale using sealed vessels but examples of microwave processing at 25 mmol scale in 125 mL of dioxane using a dedicated batch reactor is also included. If enough time, new examples of microwave-assisted Heck reactions will be included.

Coffee and Networking in Exhibition Area

11:10am

11:40am

How Can Microwave Chemistry Help the Drug Discovery Process?
Jesus Alcazar, Principal Scientist, Johnson & Johnson,
Show importance of microwave chemistry to help drug discovery programs, shorten timelines discovery of NME's.To obtain desired compounds fast and efficiently, microwaves applyed to prepare intermediates and final products at varying scale, either sequential or parallel.

Lunch and Poster Viewing

1:45pm

Keynote Address – New Chemistries by Microwave-assisted, Continuous Flow, Organic Synthesis
Michael Organ, Professor, York University
A process has been developed for the deposition of Pd black onto the inner surface of micro-capillaries and these films have been examined by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis to confirm their structure and elemental composition. These films have been shown to be highly catalytically active in metal-catalyzed transformations including the Suzuki-Miyama and Heck couplings where the reactions are flowed through these miniature capillaries while being microwaved where conversion times are in the order of seconds. Further, the role of metal films in transformations that are not specifically metal catalyzed (e.g., pericyclic reactions) has also been investigated. Here once again dramatic rate enhancements have been observed. Efforts have also been expended into differentiating OEcatalytic¹ effects from simple OEheating¹ effects for the metal film.

Coffee and Networking in Exhibition Area

3:15pm

Integrating Microwave Synthesis with Emerging Chemical Technologies
Bruce Clapham, Assistant Research Investigator, Abbott Laboratories
This talk describes the integration of our microwave synthesis platform with a newly developed high-throughput flow hydrogenation instrument.

3:45pm

Use of Microwave Reactors for Scale-up in a Kilolab
Hansjoerg Lehmann, Laboratory Head, Novartis
Results of a study about the use of microwave technology for large scale synthesis are shown, strengths and weaknesses of microwave reactors are discussed. Examples for successful scale-up are presented demonstrating significant improvements regarding reaction time and yield.

A Comparison of Sequential and Parallel Microwave Methods in the Synthesis of a Small Suzuki-Miyaura Array
Lee Schaller, Senior Scientist, GlaxoSmithKline
The use of microwaves to aid in the synthesis of organic compounds has become commonplace in many laboratories. As with many trends in organic synthesis, instrumentation has adapted to the needs of the scientist. With regards to microwave instruments, the applications appear to follow 3 different paths: Sequential, Parallel, and Constant and/or Stop-Flow technologies -- each having their own capabilities and limitations. A small array of compounds was envisioned and reaction conditions were found using conventional heating methods. These methods, although affording the desired products under the stated reaction conditions, posed a significant safety risk due to the high temperature and increased pressures. In contrast, two microwave systems, the Biotage Initiator 60 (Sequential) and Anton-Parr Synthos 3000 (Parallel), afforded the safety features, fast heating, and efficient cooling of the reactions necessary to run a small array of palladium coupling reactions. The Constant and Stop-Flow technologies were not evaluated. The current poster will compare and contrast the capabilities, limitations, and utility of these sequential and parallel microwave instruments to obtain a small array of compounds using a set of aryl bromides and aryl boronic acids/esters under Suzuki-Miyaura coupling conditions.

Drinks Reception - Compliments of Biotage

Day Two - October 4

9:00am 

Organic Synthesis - Part II
Session Chair: C. Oliver Kappe, Director, Christian Doppler Laboratory for Microwave Synthesis, University of Graz 

9:05am

Keynote Address - Priced to Sell: New Reagents for Catalysis of Heterogeneous Cross-Couplings
Bruce Lipshutz, Professor, University of California – Santa Barbara
Inexpensive nickel and copper are the base metals in groups 10 and 11, respectively, and are among the late transition metals that do most of the cross-couplings in organic synthesis. Both have been impregnated into a charcoal matrix previously and shown to catalyze various bond constructions under heterogeneous conditions. A reagent (“Cu + Ni/C”) that contains both metals within the pores in charcoal and, thus, can be used for both types of transition metal-mediated couplings will be described. New chemistry of nickel mounted between the sheets of graphite (Ni/Cg) will also be described in several ‘name’ reactions, along with comparisons between this catalyst and the corresponding reagent in charcoal (Ni/C).

9:50am

Title to be Confirmed
Luis Martinez, Assistant Professor, University of Texas – El Paso

Coffee and Networking in Exhibition Area

11:10am

From Reaction Screening to the Kilogram Lab – Microwave-assisted Synthesis in a Single Unit
Alexander Stadler, Product Manager, Anton Paar
This presentation informs about new valuable accessories for method development and parallel optimization of microwave-mediated syntheses. Highlighted is a system of sealable mirotiter plates for reaction screening.

11:40am

Advances in Microwave Assisted Organic Synthesis
Farah Mavandadi, Product Manager, Biotage
The ability to precisely control reaction conditions has encouraged chemists to include microwave technology as a standard tool in organic chemistry laboratories. This has significantly accelerated the chemical synthesis process. While the applications of microwave-assisted organic synthesis (MAOS) continue to grow, there is little emphasis on the work-up and purification of reactions, which in many instances become bottlenecks in the synthetic process. This talk will demonstrate the scope of MAOS by means of recent examples, and address the advantages of combining MAOS with solid-supported reagents and scavengers for rapid synthesis and workup of organic compounds.

Lunch and Poster Viewing

1:45pm

Microwave-Assisted Proteomics in the Biotechnology Area
Wendy Sandoval, Senior Research Associate, Genentech
Biochemical and Proteomic analysis has recently witnessed significant evolution; with more high-throughput analytical instrumentation and bioinformatic tools available, sample preparation has typically become one of the rate-limiting steps in protein characterization work-flows. Here we present on a variety of microwave-assisted reactions used for the characterization of proteins from the biotechnological arena. Many recombinant proteins that are used as bio-therapeutics possess at least one type of post translational modification. Here we present on microwave-assisted methods developed by our lab, for the removal or characterization of post-translational modifications including de-glycosylation and phosphorylation site mapping. We show how these are used in combination with other microwave-assisted biochemical techniques for the full high-throughput characterization of biotechnological drug products.

Microwave-assisted Solid-phase Peptide Synthesis
C. Oliver Kappe, Professor, University of Graz
In this lecture, the microwave-assisted solid-phase peptide synthesis of three difficult sequences will be discussed.  Using controlled microwave heating in a dedicated reactor, we have achieved the synthesis of petides that could not be synthesized using conventional automated peptide synthesizers.

Microwave Induced Thermal Gradients in Solventless Reaction Systems
Dariusz Bogdal, Professor, Politechnika Krakowska
Recently, microwave irradiation has been found to be a very efficient tool to improve yields of a great number of chemical transformations. Many authors suppose that it might be a result of specific microwave interaction with reagents on molecular scale when the reaction system polarity is increased from a ground state to a transition state or macromolecular scale, which in turn influences yield as well as selectivity. Temperature measurement during microwave irradiation of materials is the major problem in microwave-enhanced processing of materials. Applying a thermovison camera, we reported that the application of a pyrometer and fiber-optics thermometer can give incorrect values while high temperature gradients were developed within reaction mixtures. Applying a thermovision camera, we also found that for the reactions in solventless systems under microwave irradiation, the temperature measurement with a fiber-optics thermometer can lead to serious deviations like pyrometry; in particular, for those experiments that are planned without any attention paid to temperature homogeneity of the reaction mixture. In the later case, a high temperature gradient within the reaction mixture generated by microwaves leads to higher conversion of reactants or/and reaction rates.

3:15pm

Expanding the Scope of Microwave-promoted Chemistry
Nicholas Leadbeater, Professor, University of Connecticut
In this lecture, up-to-the-minute results from ongoing programs in the area of microwave-promoted chemistry will be presented. Topics covered will be: New method development for organic chemistry – in particular for reactions involving reactive gases; The scale-up of reactions for process chemistry – assessing batch and continuous processing; Development of tools for in-situ reaction monitoring including Raman spectroscopy and digital camera observation; Exploration of the use of microwave irradiation in bioscience applications.