flexiWAVE MILESTONE H E L P I N G C H E M I S T S ADVANCED FLEXIBLE MICROWAVE SYNTHESIS PLATFORM 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 latest generation of dedicated microwave reactors enables a fast screening of reaction conditions by means of parallel tests, selecting the best catalyst, solvent and conditions. Since its introduction, it has allowed chemists to run experiments faster than ever before and with higher yields. 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 flexiWAVE It is a common misconception that a laboratory microwave is just a microwave and that there are very few differences between systems. We have incorporated in the new flexiWAVE our vision of the future, our passion, and our knowledge, with the ultimate goal of helping chemists. The new Milestone flexiWAVE overcomes the limitation of conventional microwave synthesis devices, as it consists of a single microwave platform that, in combination with specific accessories, allows the chemists to perform classic glassware and high-pressure synthesis, as well as solid-phase reactions. 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”) LARGEST MICROWAVE CAVITY SOFTWARE-CONTROLLED MAGNETIC STIRRER The new Milestone flexiWAVE microwave A magnetic stirrer is built-in in the flexiWAVE cavity has a volume in excess of 70 litres, by system. far the largest currently available. It is designed to ensure vigorous stirring of Why is this important and what are the the solutions in all vessels, independently main implications of this design? on their position in the cavity, thus assuring A large cavity allows the chemist to easily reliable and consistent results. configure many different reactions setup in a very flexible environment. SAFEVIEW Starting from the classic synthesis The flexiWAVE SafeVIEW is a high glassware moving to high-pressure vessels definition digital camera interfaced with the working -alone or in parallel configuration, a instrument terminal. large cavity is also fundamental to perform It allows the chemist to monitor the solid phase synthesis tasks. progress of the chemical reaction whilst fully protected by the all-stainless steel HIGHEST MICROWAVE POWER door of the instrument. The flexiWAVE is equipped with two 950 A video of the entire run is shown in real Watt magnetrons for a total of 1900 Watt time allowing to follow the reaction and the making it the most powerful microwave additions of reagents to be followed. platform system available for organic and inorganic synthesis. USER INTERFACE The flexiWAVE is controlled via a compact MICROWAVE FIELD HOMOGENEITY terminal with an easy-to-read, bright, full-The system additionally employs a colour, touchscreen display. rotating diffuser that evenly distributes the The terminal is provided with multiple microwaves throughout the cavity. USB and Ethernet ports for interfacing the High power coupled with the diffuser instrument to external devices and to the enables very fast and homogeneous heating local laboratory network. of samples from milli-gram to multi-gram The terminal runs a completely new preparations. user-friendly, icon-driven, multi-language software to provide easy control of the BEST REACTION CONTROL microwave run. The new Milestone flexiWAVE is equipped Simply recall a previously stored method with the most advanced yet easy to use or create a new one, press ‘START’ and reaction sensors for the most complete the system will automatically follow control of the reaction process. the user defined temperature utilizing a Temperature can be monitored by fiber sophisticated PID algorithm. optic and infrared sensors. Furthermore, all reaction parameters can When performing parallel reactions, a be modified “on-the-fly”, thus assuring the contact-less sensor is used to control each highest flexibility of operation. and every vessel, and the actual temperature values are shown on the instrument control terminal, allowing an instant visual check of the reaction conditions. BUILT-IN EXHAUST SYSTEM The flexiWAVE actually acts as a relatively small fume hood, as it incorporates a powerful exhaust system, which cools the outer surface of the reactors and provides a safe and efficient removal of vapors from the microwave cavity. flexiWAVE control terminal Condenser Adapter Fiber optic temperature sensor Infrared temperature sensor 500 mL glass flask Weflon support Magnetic stirrer CLASSIC GLASSWARE The flexiWAVE has been designed and engineered as a ‘microwave platform’, where all types of commonly used • Conventional synthesis in glassware can be used. This clearly results in a very flexible system, with a wide microwave cavity range of applications capabilities. The Classic Glassware setup, for instance, provides the • Distillation suitable apparatus for a full reaction optimization, for research or teaching purposes. • Reflux It allows the chemists to perform synthetic reactions • Reagents addition under reflux and subsequently, any chemical reaction currently carried out with hot plates, heating mantles or oil • Easy sampling baths, could be rapidly improved by adopting microwave technology. Rapid preparation of pyranoquinolines using microwave dielectric heating in combination with fractional product distillation T Razzaq, C.O. Kappe, Tetrahedron Letters 2007, 48, 2513 – 2517 Fiber optic temperature sensor Rotating high-pressure carousel High-pressure 100mL vessel Infrared temperature sensor Magnetic stirrer HIGH-PRESSURE Stubborn reactions are typically carried out in refluxing conditions, using high boiling solvents such as xylenes, • High pressure and temperature 1,2-dichlorobenzene and N-methyl pyrrolidone. High boiling solvents are then difficult to remove upon • Faster reaction rate workup, especially as reaction scale increases. The High-Pressure setup is capable of replacing reflux • Switching from high boiling devices, moving from high boiling solvents to low boiling solvents. point solvents to lower one Moreover, high temperature reactions (up to 300 °C) can • Single-vessel or parallel be used. The benefits are well known and documented in terms of synthesis easier work-up and products purity. Up to 15 high-pressure vessels may be used simultaneously for parallel synthesis. Design and Synthesis of a g1b8-Cyclodextrin Oligomer: A New Platform with Potential Application as a Dendrimeric Multicarrier A. Barge et al., Chem. Eur. J. 2013, 19, 12086 – 12092 Vacuum port 45° tilted rotating glass reactor (2,5 L or 300 mL) Infrared temperature sensor SOLID-PHASE Heating heterogeneous reaction mixtures, thick media or solid phase systems suffers of inhomogeneous • Homogeneous heating of solid temperature distribution and stirring difficulties using conventional microwave instruments. mixture The innovative Solid-Phase setup offers the unique capability of physically rotating the reaction vessel, to • No wall effect achieve very homogenous bulk heating of slurries, viscous and solid reaction mixtures media. • Ease removal of volatile by- The reaction temperature is controlled by a contact-less products infrared sensor. Furthermore, the Solid-Phase setup allows operations • Solution concentration during under normal atmosphere, inert gas, and vacuum. Functionalization and modifications of materials, the reaction process polycondensation, coating, and dehydration of natural oils are some of the most common applicationsv. Efficient Green Protocols for Preparation of Highly Functionalized ß-Cyclodextrin-Grafted Silica K. Martina et al., ACS Sustainable Chem. Eng. 2014, 2, 2595−2603 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 T361EN-001 www.mls-mikrowellen.de - email: mws@mls-mikrowellen.de CA