Scientific Papers

for Microwave Assisted Synthesis with

  • flexiWAVE - Classic Glassware Configuration

    The flexiWAVE has been thought and engineered as a ‘microwave platform’, where all types of commonly used glassware could be used.
    This clearly results in a very flexible system, with a wide range of applications capabilities. The Classic Glassware setup, for instance, provides the suitable apparatus for a full reaction optimization, for research or teaching pourposes.
    It allows the chemists to perform synthetic reactions under reflux and, in this manner, any chemical reaction currently carried out with hot plates, heating mantles or oil baths, could be rapidly improved by adopting microwave technology.

"Rapid microwave-promoted synthesis of new sulfonylmethylbenzothiazoles in water"
Gellis, A., Boufatah, N., Vanelle, P., Green Chem., 2006, 8, 483–487

"Rapid preparation of pyranoquinolines using microwave dielectric heating in combination with fractional product distillation"
Razzaq, T., Kappe, C. O., Tetrahedron Letters, 2007, 48, 2513–2517

"Facile Synthesis of Optically Active Imidazole Derivatives"
Marek, A., Kulhanek, J., Ludwig, M., Bures, F., Molecules 2007, 12, 1183-1190

"Synthesis, characterization and microwave-enhanced polymerization of a phthalonitrile resin"
Selvakumar, P., Sarojadevi, M., Sundararajan, P., Materials Science and Engineering B, 2010, 168, 214–218

"Microwave-assisted template synthesis of diazacyclam-based macrocyclic copper complex and forming octahedral, square planar and square pyramidal geometries by ion exchanging and introducing a novel 2D square-grid copper–mercury coordination polymer"
Mohammad Hakimi, M., Moeini, K., Mardani, Z., Mohr, F., Polyhedron, 2014, 70, 92–100

"New cyclodextrin dimers and trimers capable of forming supramolecular adducts with shape-specific ligands"
Silvio Aime et al, Org. Biomol. Chem., 2009, 7, 370–379

"Synthesis and cytotoxicity evaluation of some benzimidazole-4,7-diones as bioreductive anticancer agents"
Gellis, A., Kovacic, H., ne Boufatah, N., Vanelle, P., European Journal of Medicinal Chemistry, 2008, 43, 1858-1864

"Synthesis and Pharmacological Evaluations of Sildenafil Analogues for Treatment of Erectile Dysfunction"
Silvio Toque, H. A. F. et al, J. Med. Chem., 2008, 51, 2807–2815

"Assisted Microwave Synthesis of High Molecular Weight Poly(ArylEtherKetone)s"
Brunel R. et al, High Performance Polymers, 2008, 20, 185–207

"The effect of microwave irradiation on carbodiimide-mediated esterifications on solid support"
Stadler, A., Kappe, C. O., Tetrahedron, 2001, 57, 3915-3920
high pressure
  • flexiWAVE - High Pressure Configuration

    Stubborn reactions are typically carried out in refluxing conditions, using high boiling solvents such as xylenes, 1,2- dichlorobenzene and N-methyl pyrrolidone. High boiling solvents are then difficult to remove upon workup, especially as reaction scale increases.
    The High-Pressure setup is capable of replacing reflux devices, moving from high boiling solvents to low boiling solvents. Moreover, high temperature reactions (up to 300 C) are allowed.
    The benefits are well known and documented in terms of easier work-up and products purity. Up to 15 high-pressure vessels may be used simultaneously for parallel synthesis.

"Towards the rehabilitation of the Mathews’ ‘dry’ hydrolysis reaction using microwave technology"
Chemat, F., Tetrahedron Letters, 2002, 43, 5555–5557

"Design and Synthesis of a g1b8-Cyclodextrin Oligomer: A New Platform with Potential Application as a Dendrimeric Multicarrier"
Barge, A. et al, Chem. Eur. J., 2013, 19, 12086 – 12092

"Novel synthetic approach in microwave-assisted solid-supported oxidations using ‘in situ’ generated molecular oxygen"
Gershonov, E., Katz, E., Karton, Y., Zafrani, Y., Tetrahedron, 2007, 63, 3762–3767

"Microwave-assisted depolymerisation of organosolv lignin via mildhydrogen-free hydrogenolysis: Catalyst screening"
Toledano, A. et al, Applied Catalysis B: Environmental, 2014, 145 43– 55

"Microwave-assisted polymerization process: A way to design new, high molecular weight poly(arylimidazole)s"
Chauveau, E., Marestin, C., Martin, V., Mercier, R., Polymer, 2008, 49, 5209–5214

"Water-borne Polyimides via Microwave-assisted Polymerization"
Brunel, R., Marestin, C., Martin, V., Mercier, R., High Performance Polymers, 2009, DOI: 10.1177/0954008308101150

"Efficient synthesis of small molecule macroarrays: optimization of the macroarray synthesis platform and examination of microwave and conventional heating methods"
Bowman, M. D. et al, Tetrahedron, 2006, 62, 4715–4727

"Microwave superheated water and dilute alkali extraction of brewers’ spent grain arabinoxylans and arabinoxylooligosaccharides"
Coelho, E., Rocha, M. A. M., Saraiva, J. A., Coimbra, M. A., Carbohydrate Polymers, 2014, 99, 415– 422

"Sequential microwave superheated water extraction of mannans fromspent coffee grounds"
Passos, C. P., Moreira, A. S. P., Dominguesa, M. R. M., Evtuguinb, D. V., Coimbra, M. A., Carbohydrate Polymers, 2014, 103, 333– 338

"Microwave superheated water extraction of polysaccharides from spent coffee grounds"
Passos, C. P., Coimbra, M. A., Carbohydrate Polymers, 2013, 94, 626–633

"Microwave-assisted hydrothermal synthesis of zeolite Beta coatings on ALD-modified borosilicate glass for application in microstructured reactors"
Muraza, O. et al, Chemical Engineering Journal, 2008, 135, 117–120

"Increased ionic conductivity in microwave hydrothermally synthesized rare-earth doped ceria Ce1−xRExO2−(x/2)"
Prado-Gonjal, J. et al, Journal of Power Sources, 2012, 209,163– 171

"Microwave advantages in inorganic synthesis of La0.5Sr0.5MnO3 powders for perovskite ceramics"
Rizzuti, A., Leonelli, C., Processing and Application of Ceramics, 2009, 3, 29–32

"Evaluation of structural transformation in 2D metal–organic frameworks based on a 4,4′- sulfonyldibenzoate linker: microwave-assisted solvothermal synthesis, characterization and applications"
Wu, C. Y. et al, CrystEngComm, 2014, 16, 9308

"Microwave-assisted synthesis and in-situ self-assembly of coaxial Ag/C Nanocables"
Yu, J. C., Hu, X., Li, Q., Zhang, L., Chem. Commun., 2005, 2704–2706
flexiWAVE - Solid Phase Configuration
  • flexiWAVE - Solid Phase Configuration

    Heating heterogeneous reaction mixtures, thick media or solid phase systems suffers of inhomogeneous temperature distribution and stirring difficulties using conventional microwave instruments.
    The innovative Solid-Phase setup offers the unique capability of physically rotate the reaction vessel, to achieve very homogenous bulk heating of slurries, viscous and solid reaction mixtures media.
    The reaction temperature is controlled by a contact-less infrared sensor.
    Furthermore, the Solid-Phase setup allows operations under normal atmosphere, inert gas, and vacuum.
    Functionalization and modifications of materials, polycondensation, coating, dehydration of natural oils are some of the most common area of application.

"CO2 hydrogenation to methanol over CuZnGa catalysts prepared usingmicrowave-assisted methods"
Cai, W., de la Piscina, P. R., Toyir,J., Homs, N., Catalysis Today, 2015, 242, 193–199

"The preparation of high-grade bio-oils through the controlled, low temperature microwave activation of wheat straw"
Budarin, V. L. et al, Bioresource Technology, 2009, 100, 6064–6068

"Transparent luminescent layers via ionic liquid-based approach to LaPO4:RE (RE=Ce, Tb, Eu) dispersions"
Buhler, G., Feldmann, C., Appl. Phys. A, 2007, 87, 631–636

"Microwave-Promoted Esterification Reactions: Optimization and Scale-Up"
Amore, K. M., Leadbeater, N. E., Macromol. Rapid Commun., 2007, 28, 473–477

"Ionic liquid-based approach to doped nanoscale oxides: LaPO4:RE (RE = Ce, Tb, Eu) and In2O3:Sn (ITO)"
Buhler, G., Stay, M., Feldmann, C., Green Chem., 2007, 9, 924–926

"Efficient Green Protocols for Preparation of Highly Functionalized β‑Cyclodextrin-Grafted Silica"
Martina, K., Baricco, F., Berlier, G., Caporaso, M., Cravotto, G., ACS Sustainable Chem. Eng., 2014, 2, 2595−2603

"Solubilization of hemicellulose and lignin from wheat straw through microwave-assisted alkali treatment"
Obermeier, I. J., Sieber, V., Faulstich, M., Schieder, D., Industrial Crops and Products, 2012, 39, 198– 203

"Microwave Heating Application To Produce Dehydrated Castor Oil"
Nezihe, A., Elif, D., Ozlem, Y., Tuncer, E. A., Ind. Eng. Chem. Res., 2011, 50, 398–403

"From Lignocellulosic Biomass to Lactic- and Glycolic-Acid Oligomers: A Gram-Scale Microwave-Assisted Protocol"
Carnaroglio, D. et al, ChemSusChem, 2015, DOI: 10.1002/cssc.201403183

"The potential of microwave technology for the recovery, synthesisand manufacturing of chemicals from biowastes"
Budarin, V. L. et al, Catalysis Today, 2015, 239, 80–89
  • 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.
    The combination of high microwave power density of 1.5kW/L and powerful stirring allows the same conditions developed for smallscale reactions to be replicated. 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.
    The synthWAVE allows for the use of a wider range of low-boiling reagents, reactants and solvents. Perform aqueous reactions and extractions below boiling point. Extremely efficient cooling of the reaction vessel avoids or minimizes degradation and side reactions. 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 CO2. Example: the preparation of isocyanates derivatives by the Staudinger-Aza-Wittig reaction.

"Functionalization of Single-Walled Carbon Nanotubes through 1,3-Cycloaddition of Carbonyl Ylides under Microwave Irradiation"
Tagliapietra, S., Cravotto, G., Calcio Gaudino, E., Visentin, S.,Mussi, V., SYNLETT, 2012, 23

"Effects of Ultrasound and Microwaves on Selective Reduction: Catalyst Preparation and Reactions"
Wu, Z., Borretto, E. Medlock, J., Bonrath, W., Cravotto, G., ChemCatChem, 2014, 6, 2762 – 2783

"Highly Efficient Microwave-Assisted CO Aminocarbonylation with a Recyclable Pd(II)/TPP-β-Cyclodextrin Cross-Linked Catalyst"
Calcio Gaudino, E. 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"
Calcio Gaudino, E. et al, Org. Biomol. Chem., 2014, 12, 4708

"Efficient microwave-assisted synthetic protocols and in silico behaviour prediction of per-substituted β- cyclodextrins"
K. Martina et al, Org. Biomol. Chem., 2013, 11, 5521

"Evaluation of the Impact of Sequential Microwave/Ultrasound Processing on the IgE Binding Properties of Pru p 3 in Treated Peach Juice"
Garino, C. et al, J. Agric. Food Chem., 2012, 60, 8755−8762

"Ultrasound- and Microwave- Assisted Preparation of Lead-Free Palladium Catalyst: Effects on the kinetics of Diphenylacetylene Semi-Hydrogenation"
Wu, Z. et al, ChemCatChem, 2015, DOI: 10.1002/cctc.201402999

"Microwave-assisted flash conversion of non-edible polysaccharides and post-harvest tomato plant waste to levulinic acid"
Tabasso, S., Montoneri, E., Carnaroglio, D., Caporaso, M., Cravotto, G., Green Chem., 2014, 16, 73

"A green approach to heterogeneous catalysis using ligand-free, metal-loaded cross-linked cyclodextrins"
Cravotto, G., Calcio Gaudino, E., Tagliapietra, S., Carnaroglio, D., Procopio, A., Green Process Synth, 2012, 1, 269–273

"Application of a Batch Microwave Unit for Scale-Up of Alkoxycarbonylation Reactions Using a Near- Stoichiometric Loading of Carbon Monoxide"
Iannelli, M. et al, Organic Process Research & Development, 2009, 13, 634–637

"From Lignocellulosic Biomass to Lactic- and Glycolic-Acid Oligomers: A Gram-Scale Microwave-Assisted Protocol"
Carnaroglio, D. et al, ChemSusChem, 2015, DOI: 10.1002/cssc.201403183

"Enabling technologies for the rapid dechlorination of polychloroarenes and PCBs"
Cravotto, G. et al, Chemosphere, 2013, 92, 299–303

"Design and Synthesis of a g1b8-Cyclodextrin Oligomer: A New Platform with Potential Application as a Dendrimeric Multicarrier"
Barge, A. et al, Chem. Eur. J., 2013, 19, 12086 – 12092

"Complementary and synergic effects of microwaves and ultrasound in metal-assisted synthesis"
Cintas, P., Carnaroglio, D., Rinaldi, L., Cravotto, G., Chimica oggi/Chemistry Today, 2012, 30

"Industrial applications of plasma, microwave and ultrasound techniques: Nitrogen-fixation and hydrogenation reactions"
Hessel, V., Cravotto, G., Fitzpatrick, P., Patil, B. S., Lang, J., Bonrath W., Chemical Engineering and Processing, 2013, 71, 19– 30

"Pd/C-catalyzed aerobic oxidative esterification of alcohols and aldehydes: a highly efficient microwaveassisted green protocol"
Caporaso, M. et al, Beilstein J. Org. Chem., 2014, 10, 1454–1461

"One-pot sequential synthesis of isocyanates and urea derivatives via a microwave-assisted Staudinger–aza- Wittig reaction"
Carnaroglio, D., Martina, K., Palmisano, G., Penoni, A., Domini, C., Cravotto, G., Beilstein J. Org. Chem., 2013, 9, 2378–2386.