Microwave assisted synthesis
gets a boost
Microwaves (MWs) are becoming increasingly popular in organic synthesis. Though the exact mechanism of action of microwaves is not fully understood, improved yields and increased reaction rates in MW reactors have substantially increased their usage in organic synthesis. Possibility of supplying milder and/or less toxic reagents in MW reactors has further added their popularity.
Anton Paar GmbH, Australia offers synthesis 3000 multimode microwave reactor for diverse organic synthesis applications in MW assisted organic synthesis (MAOS). The Synthos 3000 enables direct scalability of well-established small-scale synthesis protocols into the multi-gram scale of products within one run, offering parallel rotors with 8, 16 or 48 vessels. The highly homogeneous microwave field allows for elaboration of reactions in parallel matter for up to 48 different mixtures in one rotor. The 16-position rotor is the universal tool for MAOS under standard microwave conditions (up to 240 °C, 40 bar), whereas Rotor 8 allows you to employ extreme temperature/pressure conditions (up to 300 °C, 80 bar). The high-throughput Rotor 48MF50 is specially designed for the library generation of valuable targets in gram scale.
Due to the highly homogeneous microwave field, provided by two magnetrons, uniformity during the reaction progress is ensured, leading to excellent reproducibility. Wireless temperature control is conducted by a gas balloon thermometer immersed in one reference vessel. As an additional control system an IR sensor measures the temperature on the outer surface of any vessel from the bottom of the cavity. The built-in magnetic stirrer can further enhance reaction rates, especially when inhomogeneous mixtures are heated.
Pressure measurement is achieved simultaneously for all vessels (Rotor 8) by a unique hydraulic pressure system integrated in the rotor top plate. With Rotor 16 and Rotor 48, parameter control is accomplished by a combined pressure/temperature sensor immersed in one reference vessel.
The maximum output power of 1400 W allows efficient heating rates with even large amounts of reaction mixtures. Cooling is achieved by a forced-air cooling system, which can decrease the temperature from 280°C to ~40 °C within 20-30 minutes.
To simplify washing and cleaving steps in solid phase synthesis under microwave conditions, a special filter unit for the 100 mL vessels is available. This tool can be applied directly on the non-adhesive PTFE-TFM liners in order to carry out a whole SPOS reaction sequence without changing the vessels.
An additional gas inlet system for use with the Rotor 8 and Rotor 16 allows you to apply individual pre-pressures of up to 20 bar with either reactant or inert gas atmospheres. This simplifies the handling of air/moisture-sensitive reagents while combining the benefits of microwave heating with the effects of high-pressure conditions.
For effective heating of weakly absorbing agents, inert passive heating elements made of silicone carbide (SiC), are available. These re-useable tools enable transformations in non-polar solvents at much higher temperatures than could be usually reached by microwave irradiation.
The delivered software package provides a common solvent/reactant library for easy generation of new reaction protocols. Several standard protocols for frequently used reactions are included which can be edited for your individual needs.
With safety becoming paramount in all processes, the Synthos 3000 guarantees the highest safety standards serving various active and passive safety measures to protect users against hazards from unexpected spontaneous chemical reactions.
To protect the vessels from damage, they are equipped with metal safety disks which open in case of sudden overpressure formation. In case of a venting action, the overpressure is released by a quick opening and immediate resealing of the cavity door.
Furthermore, the software controls the microwave output by switching off the magnetron and starting the cooling system if the temperature or pressure increase exceeds the safety limit. The magnetron is protected against overheating due to reflected irradiation by an accurate double-check temperature control system.
For further information contact: Anton Paar GmbH Website: chemie.de/products/e/info/41106
Uvikon assures reliable spectroscopic measurements
Accurate and precise photometric measurements are basic and critical for analytical and research laboratories. Continuous improvement in design and performance are fast making no so earlier models of spectrophotometers look obsolete.
Kontron Lab Instruments offers Uvikon Double Beam UV/VIS Spectrophotometer for precise measurements. The optical design of Uvikon with only six reflecting elements and fully symmetrical sample and reference beams ensures maximum energy throughout for high sensitivity even at high background absorbance. Measurements can be made from 180 to 900 mm with wavelength precision + 0.025 nm and wavelength accuracy + 0.25 nm. Quick and reliable spectral measurements can be made with Uvikon at scan speed of 5-5000 nm/min and strong light less than 0.015% T.
The Uvikon® XS version with fixed slit width is a high-performance unit designed for demanding measurements. The Uvikon® XL with variable slit width and photomultiplier technology is used where highest spectral resolution combined with maximum sensitivity and linearity in the UV region is required.
The corresponding UVS Spectra Calulation Software supports all measuring methods in UV/Vis spectrophotometry and offers significant increases in productivity. From simple absorbance measurements at single wavelengths through to complex calculations from measurements at multiple wavelengths, scans with corresponding calculation or activity calculations for kinetics with samples measured in parallel – all freely configurable methods are available per mouse click. The UVS software combines ease-of-operation with optimum flexibility and complete traceability. The integrated data base links each stored data set with the method used to create the set, thus each event is uniquely traceable. Data security for the complete data base is ensured through a backup to two different pre-defined paths.
A 21CFR11 compliant version is also available as an option. This version offers a completely integrated user management with definition of access rights, a completely traceable Audit Trail together with Electronic Signature
For Further Information, Contact: Email: info@flowspek.ch