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Paulo A. Machicao Scott R. Burt Ryan K. Christensen Nathan B. Lohner J.D. Singleton Matt A. Peterson 《Tetrahedron letters》2017,58(24):2318-2321
Treatment of N-[(4-hydroxy-6-phenyl)pyrimidin-2-yl]cyanamide with 1° alkyl or arylamines in isopropyl alcohol for only 10 min at 110–120 °C under microwave conditions gave the corresponding N′-alkyl(aryl)guanidine derivatives in excellent yields (65–84%). Isolated yields were greatest when >1.0 equiv. of amines were employed, but excellent results were also obtained when aryl and alkylamines were reacted with a more atom-economical loading (1.0 equiv.; 70% and 72% ave. yields, respectively). Arylamines with either highly electron withdrawing substituents (e.g. CO2H) or pi-deficient heterocycles (e.g. variously substituted aminopyridines) did not work well under these conditions, and reaction with ureas and/or amino acids did not give detectable products. Work-up was exceedingly simple, and involved simple collection and washing of product on a sintered glass funnel. Products were obtained in analytically pure form and required approximately 1 h to prepare, start to finish. 相似文献
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This work demonstrated for the first time that myoglobin cross‐linked in polylysine films is electrochemically active at 6 °C. At 6 °C, these protein films exhibited reversible reduction/oxidation peaks which are characteristic of FeIII/FeII redox couple. The estimated current function densities (J=1.6×10?4 C/V cm2), surface concentrations (ΓT=0.10 nmol/cm2) and standard electron transfer constant (ks=13.86 s?1) at 6 °C for the data taken at a scan rate of 0.1 V/s were similar to those which were obtained at 10, 15 and 23 °C. Basically, this study shows a possible electrocatalytic application of these myoglobin/polylysine films, for example in low temperature sensing applications. 相似文献
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Gordon J. Thorogood Brendan J. Kennedy Vanessa K. Peterson Vittorio Luca 《Journal of Physics and Chemistry of Solids》2011,72(6):692-700
The structure of the defect pyrochlore NaW2O6+δ·nH2−zO after ion exchange with K, Rb, Sr or Cs for Na has been investigated using thermal analysis, solid-state nuclear magnetic resonance, laboratory X-ray and neutron diffraction methods. Neutron diffraction studies show that both the A-type cations (Na+, K+, Rb+, and/or Cs+) and the water molecules reside within the channels that form in the 111 direction of the W2O6 framework and that these strongly interact. The analytical results suggest that the water and A-type cations compete for space in the tunnels within the W2O6 pyrochlore framework, with the total number of water molecules and cations being approximately constant in the six samples investigated. The interplay between the cations and water explains the non-linear dependence of the a lattice parameter on the choice of cation. It appears that the ion-exchange capacity of the material will be controlled by the amount of water initially present in the sample. 相似文献
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William J. Durand Andrew A. Peterson Felix Studt Frank Abild-Pedersen Jens K. Nørskov 《Surface science》2011,605(15-16):1354-1359
Polycrystalline copper electrocatalysts have been experimentally shown to be capable of reducing CO2 into CH4 and C2H4 with relatively high selectivity, and a mechanism has recently been proposed for this reduction on the fcc(211) surface of copper, which was assumed to be the most active facet. In the current work, we use computational methods to explore the effects of the nanostructure of the copper surface and compare the effects of the fcc(111), fcc(100) and fcc(211) facets of copper on the energetics of the electroreduction of CO2. The calculations performed in this study generally show that the intermediates in CO2 reduction are most stabilized by the (211) facet, followed by the (100) facet, with the (111) surface binding the adsorbates most weakly. This leads to the prediction that the (211) facet is the most active surface among the three in producing CH4 from CO2, as well as the by-products H2 and CO. HCOOH production may be mildly enhanced on the more close-packed surfaces ((111) and (100)) as compared to the (211) facet, due to a change in mechanism from a carboxyl intermediate to a formate intermediate. The results are compared to published experimental data on these same surfaces; the predicted trends in voltage requirements are consistent between the experimental and computational data. 相似文献
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A method is described for the determination of urinary 4,4'-methylenedianiline (MDA) by high-performance liquid chromatography (HPLC). MDA was extracted from hydrolyzed urine using C18 solid-phase extraction columns. The extract was analyzed by reversed-phase HPLC with electrochemical detection at a cell potential of 0.8 V. The method was very sensitive (detection limit 2.5 micrograms/l) and quantitation using 4,4'-ethylenedianiline as an internal standard correlated well with results by gas chromatography-mas spectrometry. Run-to-run precision (n = 25) averaged 8.9%. In analysis of more than 160 potentially exposed workers, MDA was detected in less than 20% of the urines and concentrations ranged up to 210 micrograms MDA per g of creatinine. 相似文献