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An environmentally friendly chemical reaction that does not waste any atoms

In the Research Group of Nuno Maulide, a chemist working at the University of Vienna, a new chemical synthesis for α-arylated Carbonyl derivatives was developed. Members of this class of substances typically possess interesting biological and pharmacological properties and often find applications as medicines. The new technique developed by the Maulide group, which allows such Carbonyl derivatives to be generated easily, efficiently and in an environmentally friendly manner – without wasting any atoms –, has raised significant scientific interest and awareness. The corresponding publication in the journal Angewandte ChemieInternational Edition was considered by the Editorial office as “highly important”.

From accidental discovery to rational design
In Organic Chemistry one often encounters surprising experimental results, e.g. when new properties of compounds or new chemical reactions are unexpectedly discovered. The discovery of a new type of reactivity, i.e. the ability of a chemical substance to undergo a new type of reaction, can shine light on unforeseen and previously unknown interesting properties of that substance. Ideally, the chemist can then make use of the unexpected result and information to develop new transformations. The phenomenon whereby a scientist can make use of an unexpected result is often termed “Serendipity”.
“Our initial, accidental discovery was an unusual transformation of amides – chemical substances that derive formally from the union of ammonia and carboxylic acids. In our current work, the addition of an activating agent generates a reactive intermediate, which subsequently undergoes an elegant rearrangement. During this rearrangement, the atomic constitution of the molecule is altered with atoms effectively changing place in a harmonious manner, leading to an entirely different product. We took advantage of the knowledge gained during that reaction for the development of the current Acid-catalysed Redox-Arylation. In other words, the information obtained during the study of that unexpected transformation allowed us to design novel useful transformations”, says Nuno Maulide, since October 2013 Full Professor for Organic Synthesis at the University of Vienna. Maulide had published that original discovery in 2010 in the journal “Angewandte Chemie”.

New: only a catalyst is needed, and no additional reagents
In most organic chemical reactions a modification of the oxidation stage of the reagents takes place. Oxidations increase the oxidation state, whereas reductions decrease that oxidation state. Both types of reactions require the addition of an external reagent, either an oxidant or a reductant. In the new family of so-called “Redox-neutral”, both steps – oxidation and reduction – take place simultaneously and concomitantly with the desired transformation. This renders additional reagents unnecessary. “The arylation that we have just developed requires only a catalyst; no other reagents are required”, explains Langui Xie, co-author of the current publication and Post-Doc in the very international group of Nuno Maulide at the University of Vienna.

Sustainability: no atoms are wasted
New methods of synthesis for arylated Carbonyl derivatives are of considerable interest for the scientific community – not least due to the very important biological activities of α-arylated carbonyls and their possible applications as medicines. Up to now, most methods employed for their preparation employed Transition-metal catalysed reactions, with the use of heavy metal reagents. This involves inevitable disadvantages such as product contamination, high catalyst costs and laborious and work-intensive reaction conditions. “The new transformation we developed requires no metals and belongs to the group of ‘Atom-economical reactions’. Such transformations are notable in that all of the atoms of the reagents are expressed in the final products; thus, no atoms are wasted during the process”, concludes the chemist Nuno Maulide.
University of Vienna


Arizona State University scientists take steps to unlock the secrets to the fountain of youth

ASU scientists, together with collaborators from the Chinese Academy of Sciences in Shanghai, have published, in Nature Structural and Molecular Biology, a first of its kind atomic level look at the enzyme telomerase that may unlock the secrets to the fountain of youth.
Telomeres and the enzyme telomerase have been in the medical news a lot recently due to their connection with aging and cancer. Telomeres are found at the ends of our chromosomes and are stretches of DNA which protect our genetic data, make it possible for cells to divide, and hold some secrets as to how we age –and also how we get cancer.
An analogy can be drawn between telomeres at the end of chromosomes and the plastic tips on shoelaces: the telomeres keep chromosome ends from fraying and sticking to each other, which would destroy or scramble our genetic information.
Each time one of our cells divides its telomeres get shorter. When they get too short, the cell can no longer divide and it becomes inactive or dies. This shortening process is associated with aging, cancer and a higher risk of death. The initial telomere lengths may differ between individuals. Clearly, size matters!
“Telomerase is crucial for telomere maintenance and genome integrity,” explains Julian Chen, professor of chemistry and biochemistry at ASU and one of the project’s senior authors. “Mutations that disrupt telomerase function have been linked to numerous human diseases that arise from telomere shortening and genome instability.”
Chen continues that, “Despite the strong medical applications, the mechanism for telomerase holoenzyme (the most important unit of the telomerase complex) assembly remains poorly understood. We are particularly excited about this research because it provides, for the first time, an atomic level description of the protein-RNA interaction in the vertebrate telomerase complex.”
Arizona State University


UC research tests which nano system works best in killing cancer cells

New UC research tested four iron-oxide nanoparticle systems to see which, when heated, would likely work best as a tool for targeting cancer cells.
In current research related to improving cancer treatments, one promising area of research is the effort to find ways to selectively pinpoint and target cancer cells while minimizing effects on healthy cells.
In that effort, it’s already been found in lab experiments that iron-oxide nanoparticles, when heated and then applied specifically to cancer cells, can kill those cells because cancer cells are particularly susceptible to changes in temperature. Increasing the temperature of cancer cells to over 43 degrees Celsius (about 109 degrees Fahrenheit) for a sufficient period of time can kill those cells.
So, a University of Cincinnati-led team – along with researchers at Iowa State University, the University of Michigan and Shanghai Jiao Tong University – recently conducted experiments to see which iron-oxide nanoparticle configurations or arrangements might work best as a tool to deliver this killing heat directly to cancer cells, specifically to breast cancer cells. The results were presented at the March 3-7 American Physical Society Conference in Denver by UC physics doctoral student Md Ehsan Sadat.
In systematically studying four distinct magnetized nanoparticle systems with different structural and magnetic properties, the research team found that an unconfined nanoparticle system, which used an electromagnetic field to generate heat, was best able to transfer heat absorbed by cancer cells.
So, from the set of nano systems studied, the researchers found that uncoated iron-oxide nanoparticles and iron-oxide nanoparticles coated with polyacrylic acid (PAA) – both of which were unconfined or not embedded in a matrix – heated quickly and to temperatures more than sufficient to kill cancer cells.

  • Uncoated iron-oxide nanoparticles increased from a room temperature of 22 degrees Celsius to 66 degrees Celsius (about 150 degrees Fahrenheit).
  • Iron-oxide nanoparticles coated with polyacrylic acid (PAA) heated from a room temperature of 22 degrees Celsius to 73 degrees Celsius (about 163 degrees Fahrenheit).

The goal was to determine the heating behaviours of different iron-oxide nanoparticles that varied in terms of the materials used in the nanoparticle apparatus as well as particle size, particle geometry, inter-particle spacing, physical confinement and surrounding environment since these are the key factors that strongly influence what’s called the Specific Absorption Rate (SAR), or the measured rate at which the human body can absorb energy (in this case heat) when exposed to an electromagnetic field.
According to Sadat, “What we found was that the size of the particles and their anisotropic (directional) properties strongly affected the magnetic heating achieved. In other words, the smaller the particles and the greater their directional uniformity along an axis, the greater the heating that was achieved.”
He added the systems’ heating behaviours were also influenced by the concentrations of nanoparticles present. The higher the concentration of nanoparticles (the greater the number of nanoparticles and the more densely collected), the lower the SAR or the rate at which the tissue was able to absorb the heat generated.

View of unconfined, uncoated iron-oxide nanoparticles as seen via a transmission electron microscope. These nanoparticles, when heated, can be applied to cancer cells in order to kill those cells.
The four systems studied
The researchers studied

  • uncoated iron-oxide nanoparticles
  • iron-oxide nanoparticles coated with polyacrylic acid (PAA)
  • a polystyrene nanosphere with iron- oxide nanoparticles uniformly embedded in its matrix
  • a polystyrene nanosphere with iron-oxide nanoparticles uniformly embedded in its matrix but with a thin film surface of silica 
  • All four nanoparticle systems were exposed to the same magnetic field for 35 minutes, and temperature measurements were performed at two-minute intervals. 
  • As stated, the PAA iron-oxide and the uncoated iron-oxide samples showed the highest temperature change. The lowest temperature changes, insufficient to kill cancer cells, were exhibited by 
  • The polystyrene nanosphere, which heated to 36 degrees Celsius (about 96 degree Fahrenheit).
  • The polystyrene nanosphere with a silica coating heated to 40 degrees Celsius (104 degrees Fahrenheit).

Support for this research was provided by a National Science Foundation grant under contract number NSF (1343568) titled “Development of Nanotechnology Minor Focused on Nano Biomedicine and Sustainable Energy.” Work at the Ames Laboratory was supported by the United States Department of Energy, Basic Energy Sciences, Division of Materials Sciences and Engineering.
University of Cincinnati


Graphene only as strong as weakest link

There is no disputing graphene is strong. But new research by Rice University and the Georgia Institute of Technology should prompt manufacturers to look a little deeper as they consider the miracle material for applications.
The atom-thick sheet of carbon discovered this century is touted not just for its electrical properties but also for its physical strength and flexibility. The bonds between carbon atoms are well known as the strongest in nature, so a perfect sheet of graphene should withstand just about anything. Reinforcing composite materials is among the material's potential applications.
But materials scientists know perfection is hard to achieve. Researchers Jun Lou at Rice and Ting Zhu at Georgia Tech have measured the fracture toughness of imperfect graphene for the first time and found it to be somewhat brittle. While it's still very useful, graphene is really only as strong as its weakest link, which they determined to be "substantially lower" than the intrinsic strength of graphene.
"Graphene has exceptional physical properties, but to use it in real applications, we have to understand the useful strength of large-area graphene, which is controlled by the fracture toughness," Zhu said.
The researchers reported in the journal Nature Communications the results of tests in which they physically pulled graphene apart to see how much force it would take. Specifically, they wanted to see if graphene follows the century-old Griffith theory that quantifies the useful strength of brittle materials.
It does, Lou said. "Remarkably, in this case, thermodynamic energy still rules," he said.
Imperfections in graphene drastically lessen its strength – with an upper limit of about 100 gigapascals (GPa) for perfect graphene previously measured by nanoindentation – according to physical testing at Rice and molecular dynamics simulations at Georgia Tech. That's important for engineers to understand as they think about using graphene for flexible electronics, composite material and other applications in which stresses on microscopic flaws could lead to failure.
The Griffith criterion developed by a British engineer during World War I describes the relationship between the size of a crack in a material and the force required to make that crack grow. Ultimately, A.A. Griffith hoped to understand why brittle materials fail.
Graphene, it turns out, is no different from the glass fibers Griffith tested.
"Everybody thinks the carbon-carbon bond is the strongest bond in nature, so the material must be very good," Lou said. "But that's not true anymore, once you have those defects. The larger the sheet, the higher the probability of defects. That's well known in the ceramic community."
A defect can be as small as an atom missing from the hexagonal lattice of graphene. But for a real-world test, the researchers had to make a defect of their own – a pre-crack – they could actually see. "We know there will be pinholes and other defects in graphene," he said. "The pre-crack overshadows those defects to become the weakest spot, so I know exactly where the fracture will happen when we pull it.
"The material resistance to the crack growth – the fracture toughness – is what we're measuring here, and that's a very important engineering property," he said.
Just setting up the experiment required several years of work to overcome technical difficulties, Lou said. To suspend it on a tiny cantilever spring stage similar to an atomic force microscopy (AFM) probe, a graphene sheet had to be clean and dry so it would adhere (via van der Waals force) to the stage without compromising the stage movement necessary for the testing. Once mounted, the researchers used a focused ion beam to cut a pre-crack less than 10 percent of the width into the microns-wide section of suspended graphene. Then they pulled the graphene in half, measuring the force required.
While the Rice team was working on the experiment, Zhu and his team performed computer simulations to understand the entire fracture process.
"We can directly simulate the whole deformation process by tracking the motion and displacement with atomic-scale resolution in fairly large samples so our results can be directly correlated with the experiment," said Zhu. "The modeling is tightly coupled with the experiments."
The combination of modeling and experiment provides a level of detail that allowed the researchers to better understand the fracture process – and the tradeoff between toughness and strength in the graphene. What the scientists have learned in the research points out the importance of fabricating high-quality graphene sheets without defects, which could set the stage for fracture.
"Understanding the tradeoff between strength and toughness provides important insights for the future utilization of graphene in structural and functional applications," Zhu added. "This research provides a foundational framework for further study of the mechanical properties of graphene."
Lou said the techniques they used should work for any two-dimensional material. "It's important to understand how defects will affect the handling, processing and manufacture of these materials," he said. "Our work should open up new directions for testing the mechanical properties of 2-D materials."
Rice University


Asynt has developed a version of DrySyn heating block purpose designed to allow scientists to perform safe, productive heating and stirring experiments with pear shaped flasks commonly used with rotary evaporators. Pear shaped flasks are popular with organic chemists as concentrated samples can be removed much more easily than from a round bottom flask. Pear-shaped flasks are used for evaporating solutions to dryness post synthesis using a rotary evaporator, the “rounded V” shape of the flasks enables solid materials to be scraped out more efficiently than from a round bottomed flask. Martyn Fordham, Managing Director of Asynt commented: “By designing a version of the DrySyn to accept these flasks - chemists can now eliminate the need for sample transfers between reaction flask and an evaporator (pear-shaped) flask, allowing the same flask to be used for both Synthesis and Evaporation”. Made of chemically resistant, anodized aluminium, the DrySyn range of heating blocks for pear-shaped flasks (100mL, 250ml, 500mL, 1000mL) offer excellent heating performance to over 300ºC and can heat a reaction flask 25 per cent faster than an oil bath. Providing excellent heating and stirring performance but without the inherent risks and mess of an oil bath, DrySyn heating blocks help laboratory scientists create a safer, cleaner and more efficient working environment. DrySyn heating blocks also offer a flexible, safe alternative to using heating mantles.


Sygnature Discovery (Nottingham, UK) has been using an Asynt DrySyn SnowStorm system to perform low temperature reactions which have traditionally been difficult to undertake reproducibly on a small to medium scale. The Asynt DrySyn SnowStorm offers an attractive solution to laboratories undertaking low temperature reaction chemistries. Available in a choice of configurations, the DrySyn SnowStorm system provides controlled cooling and heating for sub-ambient parallel chemistry without the need for jacketed reaction vessels, or ice baths. Operating with a suitable chiller / circulator, a DrySyn SnowStorm system provides accurate, stable temperature control down to -50 °C and up to +150 °C. Dr Geraint Jones, Associate Director of Chemistry at Sygnature Discovery commented: "Being able to maintain a sub-ambient temperature sometimes for significant periods is really important for reaction reproducibility. The DrySyn SnowStorm connects to an external chiller unit and holds temperatures at a set-point for as long as is required. Setting temperature ramping profiles is also possible which is important in optimisation studies and is a real added benefit to us". His colleague Mark Mills, Senior Research Chemist at Sygnature Discovery added: "We purchased the DrySyn SnowStorm to achieve tight temperature control (at -20°C) for a reaction involving a stereoselective cyclisation. If we had not been able to maintain this temperature for a sustained period, racemisation could have occurred. We selected this Asynt equipment because it integrated well into our way of working and allowed the use of round-bottomed flasks in a variety of sizes, thereby providing the flexibility to conduct small to medium scale reactions".


Perstorp’s ongoing commitment to the Americas includes future manufacturing investments in the region, and extensive global support for American customers. The company has established itself as a world leader in all its focus areas. David Wolf, Perstorp’s Region Head Americas refers: “Having been a manufacturer for nearly 40 years in the Americas Perstorp is well aware of the energy competitiveness of the region, and that is a strong factor in favour of new manufacturing investments”. The company recently increased its global capacity of core products, such as Capa™ and Neopentyl Glycol, in its desire to pursue new growth opportunities through partnerships with key American regional and global customers. Perstorp is the world leader in caprolactones polyol and thermoplastic technology supplied under the Capa™ brand name.

Novasep has announced its unaudited consolidated results for the period ended December 31st, 2013. The company is excited by the performance achieved through the year including: -8 percent revenue growth, reaching €316m; -15 percent EBITDA growth and increase of almost €5m and reaching €38.5m, meaningfully ahead of investor guidance for the year; -improvement in performance in every division of the business; -net cash flow from operations of €16m, from €6m in 2012; -on-time and on-target performance in its key customer commitments, including the building of the largest chromatography plant in Mourenx, expected to be operational during summer 2014.


Aptar Pharma Prescription Division recently presented and discussed the latest data from a number of user studies carried out with its Pro-Ject® auto-injector. Aptar Pharma’s Pro-Ject® is a novel auto-injector that has been designed and developed with input from patients and healthcare professionals to provide optimal patient convenience and compliance. Gerallt Williams, Director Scientific Affairs, Aptar Pharma Prescription Division explains: “Patient-centric development of drug delivery devices is now the accepted norm. Applying Human Factor principles means that the outcomes should benefit all the stake-holders involved […] Aligning Pro-Ject® with patient needs during its development process is a major step forward in delivering this benefit”.


Previously supported by Mettler Toledo, the MiniBlock® product line is now manufactured and supplied by SiliCycle Inc. The SiliCycle MiniBlock® platform enables solution phase synthesis, solid phase & peptide synthesis, and parallel purification. The flexibility of its design allows chemists to rapidly configure this compact parallel reactor to fit the needs of their chemistry, whether it requires inert conditions, refluxing or cooling. SiliCycle MiniBlock® also offers fast bottom filtration without having to invert or disassemble the reactor. Rapid purification and filtration can be achieved by stacking two SiliCycle MiniBlocks® and using SPE techniques to remove excess reagents, side-products, catalysts and metals. Taking advantage of SiliCycle’s exceptionally broad portfolio of scavengers, for both metallic and organic impurities, chemists can perform synthesis and purification on a single platform.


Waters UltraPerformance Convergence Chromatography™ [UPC2®] System combines the best features of LC and GC: higher selectivity via orthogonal modes of separation and higher mobile-phase diffusion and efficiency, respectively. Scientists now may handle both routine and challenging separations with a level of reliability, robustness, sensitivity, and throughput never before achieved when using a dense gas (supercritical fluid) as a mobile phase. When adequately compressed and made dense, carbon dioxide (CO2) becomes a “green”, environmentally sustainable, non-toxic, inexpensive alternative to expensive HPLC-grade solvents, especially those toxic organic liquids that incur significant disposal costs. As the primary UPC2 mobile phase, its low viscosity may decrease operating pressure while increasing efficiency for a given particle size and linear velocity. Compared to LC solvents, mass transfer in supercritical-fluid CO2 is enhanced. Its critical temperature (31°C) is far lower than typical GC operating temperatures, so, as with LC, heat-labile compounds may be analyzed. UPC2 technology exploits the orthogonality of normal-phase LC versus reversed-phase LC. It has the potential to separate a wider polarity and structural range of analytes: acidic, basic, and neutral compounds, lipophilic and hydrophilic solutes, stereoisomers, diastereomers, and enantiomeric or chiral compounds.


Merck Millipore, the Life Science division of Merck, has announced a new non-exclusive, preferred distribution agreement for Western Europe with VWR a global provider of laboratory supplies, equipment and services. The contract includes a range of Merck Millipore products and reagents for chemical and microbiological analysis, which are mainly used in quality control solutions for the pharmaceutical, food and beverage and chemical industries, as well as products for research in the field of organic synthesis and biosciences. “The new contract continues an important relationship with one of Merck Millipore’s largest distributors and reinforces our commitment to providing our existing customers easy access to high quality products” notes Robert Yates, Head of Merck Millipore and adds: “We will give VWR access to more Merck Millipore products and expect with VWR’s wide geographic coverage across Western Europe we will be able to reach a larger customer base”.


Clariant and Ashland Inc. have announced that they have entered into a definitive agreement to sell their joint venture, ASK Chemicals headquartered in Hilden, Germany, to investment funds affiliated with Rhône, a London and New York-based private equity investment firm. The transaction is expected to close during the third quarter 2014 and is subject to customary closing conditions, including regulatory approvals. Hariolf Kottmann, CEO of Clariant refers: “The divestment of our stake in ASK Chemicals is part of our continuous active portfolio management to reallocate capital towards our more profitable growth areas […] In the joint venture we have successfully combined the activities of Ashland and former Süd-Chemie businesses. Now we release it to a new owner who will focus on growth perspectives”.


W. R. Grace & Co. has announced the launch of ProVance™ pre-packed Protein A columns at Bioprocessing Development Week in San Diego, CA USA and the Bioprocess International Conference in Prague, Czech Republic. ProVance™ columns are a high-performance disposable chromatography solution to help meet the growing demand for downstream purification. Until now, there has not been a cost-effective Protein A chromatography option for single-use manufacturing facilities. ProVance™ columns combine Grace proprietary incompressible silica with cost-effective Protein A and disposable column hardware. The high capacity columns can reduce operating costs by 40-60 percent and are ideally suited for single-batch or single-campaign use eliminating the need for significant cleaning validations and long-term storage.


The Food and Drug Administration (FDA) has accepted the proposal made by PharmaMar, of the Zeltia Group for the production process of PM1183, a new anti-tumour agent, in clinical development for the treatment of haematological and solid tumours. The starting materials for the initiation of the production process have also been approved. Approval from the FDA confirms the strategy PharmaMar has established for the production process of PM1183, a process that is already fully defined.


Multiwave GO represents a masterstroke of Anton Paar's engineering. Multiwave GO is a routine digestion system with an extremely lightweight rotor for 12 vessels providing SMART VENT technology. Based on a DMC Directed Multimode Cavity - the new self-adjusting microwave field invented by Anton Paar - highly efficient heating is possible in an extremely small-footprint system. For efficient reaction control the internal vessel temperature of each vessel is controlled via an IR sensor.


“In 2014, we are aiming to further expand the agrochemicals segment, actively develop attractive projects in the animal health segment and strengthen business with selected multi-customer products. We are also looking to attract new customers from the specialty chemicals segment to our portfolio” says Wolfgang Schmitz, Managing Director of Saltigo GmbH, summarizing the company's plans. India is a rapidly expanding market in the field of agrochemicals. “We can support this forecast growth in custom manufacturing in particular, as this is our core competence” has added Schmitz.


Shimadzu introduces its LabSolutions chromatography software with integrated data management for workstation or network use. This new release of the LabSolutions DB and CS version completes the chromatography software family with a database embedded stand-alone and a database assisted Client / Server software package. It is an easy-to-use interface offering remote analysis operation without any special software requirement. Users benefit from advanced server, database, project, security and user management. Using the functions of the Windows terminal server and Citrix, LabSolutions when installed on a terminal server enables use on a client PC without LabSolutions (S/W). This reduces validation and S/W update work significantly. Using the Citrix XenApp, it is also possible to operate the LabSolutions software on an iPad.


Dolomite has launched Mitos Dropix, an ingenious droplet-on-demand system capable of easily generating extremely miniaturised droplet compartments with exceptional control over volume, environment and isolation of contents. Meeting the increasing demand for screening massive numbers of biological reactions, increased speed of screening and reduced reagent consumption, Mitos Dropix technology now introduces liquid sampling and processing over a very wide 10 nL – 50 μL volume range utilizing droplet technology. Mitos Dropix will be invaluable to application areas such as droplet library creation, cell encapsulation, diagnosis screening, synthetic chemistry and drug bioassays, as well as being applicable to high-throughput screening formats.


After three record-breaking years in a row, Drägerwerk AG & Co. KGaA achieved stable order intake and net sales development in fiscal year 2013. Order intake fell by 0.9 percent to EUR 2,384.6 billion (2012: EUR 2,405.5 billion). At EUR 2,374.2 billion, net sales were on previous year’s level (2012: EUR 2,373.5 billion). However, net of currency effects, order intake rose by 2.2 percent and net sales by 3.1 percent. The reason for this is the considerable increase in the strength of the euro compared to many emerging-market currencies, and also in relation to currencies such as the Japanese yen. Net sales increased in Germany in 2013, while the rest of Europe saw a decline net of currency effects. In the Asia/Pacific and Americas regions, Dräger increased its net sales adjusted for currency effects. In the Asia/Pacific region, but also in Africa and the Middle East significant growth was achieved.


BASF has received the EXCiPACT™ Certificate for pharmaceutical excipients for the group of polyvinylpyrrolidone (Kollidon®) polymers, produced in Ludwigshafen. The certificate was issued by mdc medical device certification GmbH - one of EXCiPACT’s internationally-recognized Certification Bodies. “BASF is the third company which has been certified by EXCiPACT” said Dr. Iain Moore, Chairman of the EXCiPACT Association’s Global Steering Committee and continued: “With the certificate we minimize risks for customers and help ensure patient safety while reducing costs”.