synthWAVE MILESTONE H E L P I N G C H E M I S T S THE GAME CHANGER IN MICROWAVE SYNTHESIS THE BENEFITS OF MICROWAVE TECHNOLOGY Microwave technology is changing the way to design and optimize synthetic protocols as well as their scaling up to multi-gram production. The last generation of dedicated microwave reactors enables a fast screening of reaction conditions by means of parallel tests, selecting best catalyst, solvent and conditions. Since its introduction, it has allowed to run experiments faster than ever before and with higher yield. Today microwave assisted synthesis has become a cutting-edge technology across the pharmaceutical, biotech, polymers, fine- and agro-chemical industries, with thousands of units installed worldwide. MILESTONE synthWAVE The new Milestone synthWAVE is designed for safe, reliable and reproducible scale-up of microwave-enhanced chemical reactions. It handles single or multiple reactions at temperatures up to 300 °C and pressures to 199 bar. Small-scale synthesis methods are easily transferred to the synthWAVE. Incredibly easy to use, the synthWAVE allows the chemist to run large-scale batch and parallel reactions like never before. REACTIONS COMPLETED IN MINUTES INSTEAD OF HOURS ENHANCED SELECTIVITY IMPROVED YIELDS LOWER BY-PRODUCTS FORMATION AND SAMPLE CONTAMINATION REDUCED ENERGY CONSUMPTION REDUCED QUANTITY OF SAMPLE/CHEMICALS (“ATOM ECONOMY”) SRC TECHNOLOGY Milestone’s unique Single 4 Reaction Chamber (SRC) technology overcomes the limitations of current microwave synthesis instrumentation. At the heart of the synthWAVE is a PTFE lined, 1 L stainless steel reaction chamber, which is also the microwave cavity. 1 This allows the design of the microwave source to be 3 perfectly matched to the cavity shape for optimum 2 microwave distribution and fast, even heating. The chamber is pre- pressurized with gas to prevent boiling of the solution, and is equipped with mechanical and magnetic stirrers. The microwave cavity is water cooled, which greatly reduces USER INTERFACE reaction cooling time and stored method or create a increases productivity. new one, press ‘START’ and Reaching up to 300 °C and the system will automatically 199 bar, the synthWAVE is follow the user defined capable of higher temperature temperature utilizing a and pressure than any other sophisticated PID algorithm. microwave system. Furthermore, all reaction parameters can be modified SAFETY “on-the-fly”, thus assuring the Like all Milestone products, The synthWAVE is controlled highest flexibility of operation. the synthWAVE has been via a compact terminal with designed with operator safety an easy-to-read, bright, full- SOFTWARE-CONTROLLED STIRRER of paramount importance. colour, touchscreen display. A thick acrylic shield surrounds The terminal is provided with the work area, and it lowers multiple USB and Ethernet into position automatically as ports for interfacing the the chamber is closed. instrument to external devices A microwave run cannot be and to the local laboratory started unless the chamber network. clamp is in position, and the The terminal runs a clamp cannot be released completely new user-friendly, until the chamber is cool, and icon-driven, multi-language pressure has been released. software to provide easy The synthWAVE features a The PID controller control of the microwave run. powerful stirrer, which ensures continuously monitors Simply recall a previously vigorous stirring temperature and pressure, in the 1L PTFE vessel, or in all instantaneously adjusting vials whenever a rack is used, microwave power to control thus assuring reliable and even highly exothermic consistent results. reactions. HOW THE synthWAVE WORKS Acrylic safety shield Overhead stirrer In-situ sampling Gas outlet Gas inlet Gas release valve Analog pressure gauge 15-place rack Exhaust system Temperature sensor Clamps PTFE 1 L vessel Dewar flask Control terminal FEATURES AND BENEFITS RACK AND VIALS EASY SCALE-UP Reactions can be carried out directly in the 1L The combination of high microwave power PTFE vessel, or in multiple vials. density of 1.5kW/L and powerful stirring allows Vials are available in glass (disposable), quartz the same conditions developed for small-or PTFE, fitted with loose PTFE caps to ensure scale reactions to be replicated. pressure equalization. Available rack configurations include 4, 5, 15 and 22 positions. Numbered rack trays give the operator an easy visual check of vial number. The synthWAVE sample racks fit easily on a balance, so reagents can be weighed directly into vials already loaded into a rack. No vessel assembly or disassembly is required, and with the disposable glass vials, no cleaning step is needed, greatly increasing FASTER SCREENING work efficiency. Multiple reactions are carried out simultaneously under exactly the same temperature and pressure conditions - even using different solvents. Quickly and easily evaluation of different catalysts, solvents and reaction conditions. HIGH PRESSURE CAPABILITY The synthWAVE allows for the use of a wider EASY SAMPLING range of low-boiling reagents, reactants and Easily and conveniently sample reaction solvents. products at any time during the experiment. Perform aqueous reactions and extractions below boiling point. Extremely efficient cooling of the reaction vessel avoids or minimizes degradation and side reactions. OPERATE IN MODIFIED CONDITIONS Simply add an inert gas to achieve an inert environment. Add hydrogen or oxygen to produce a reducing or oxidizing atmosphere respectively. Speed up reactions with gas molecule insertion using gases such as CO or CO .2 Example: the preparation of isocyanates derivatives by the Staudinger-Aza-Wittig reaction. APPLICATIONS • Oxidations and Reductions • Cycloadditions • Esterification & Ammidation • Reagents and Materials • Coating • Click chemistry • Polymerization • Gas insertion • Nanoparticles preparation • Multicomponent reactions • Modification of carbon nanotubes • Dechlorination • Reactions with sensitive reagents • Subcritical fluids extracion and materials • Stereoselective transformations • Desulphurization • C-C, C-X Couplings One-pot sequential synthesis of isocyanates and urea derivatives via a microwave-assisted Staudinger–aza- Wittig reaction D. Carnaroglio et al., Beilstein J. Org. Chem., 2013, 9, 2378-2386 Pd/C-catalyzed aerobic oxidative esterification of alcohols and aldehydes: a highly efficient microwave-assisted green protocol M. Caporaso et al., Beilstein J. Org. Chem. 2014, 10, 1454–1461 Highly Efficient Microwave-Assisted CO Aminocarbonylation with a Recyclable Pd(II)/TPP-ß-Cyclodextrin Cross-Linked Catalyst E. Calcio Gaudino et al., Org. Process Res. Dev. 2015, DOI: 10.1021/op5003374 A novel SWCNT platform bearing DOTA and β-cyclodextrin units. “One shot” multidecoration under microwave irradiation E. Calcio Gaudino et al., Org. Biomol. Chem. 2014, 12, 4708- 4715 HELPING CHEMIST Milestone has been active since 1988 in the field of microwave sample preparation. With over 20000 instruments installed worldwide, we are the acknowledged industry leader in microwave technology. Milestone vision is to help chemists by providing the most technologically advanced instrumentation for research and quality control. Our products offer a wide range of applications, such as microwave acid digestion, solvent extraction, synthesis and ashing. Furthermore we create products for acid purification and direct mercury determination in solid, liquid and gas samples. We offer our customers the highest level of application support, building up over the years a relationship based on trust and commitment. MILESTONE MILESTONE Srl - Via Fatebenefratelli, 1/5 - 24010 Sorisole (BG) - Italy Tel: +39 035 573857 - Fax: +39 035 575498 www.milestonesrl.com - email: analytical@milestonesrl.com MILESTONE INC. - 25 Controls Drive - Shelton, CT 06484 - USA Tel: (203) 925-4240 - Toll-free: (866) 995-5100 - Fax: (203) 925-4241 H E L P I N G www.milestonesci.com - email: mwave@milestonesci.com C H E M I S T S MILESTONE GENERAL K.K. - KSP, 3-2-1, Sakado - Takatsu-Ku, Kawasaki 213-0012 - Japan - Tel: +81 (0)44 850 3811 - Fax: +81 (0)44 819 3036 UNI EN ISO 9001: 2008 CERTIFIED www.milestone-general.com - email: info@milestone-general.com MLS GmbH - Auenweg 37 D-88299 Leutkirch im Allgau - Germany Tel: +49 (0)7561 9818-0 - Fax: +49 (0)7561 9818-12 T333EN-002 www.mls-mikrowellen.de - email: mws@mls-mikrowellen.de CA