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11.
The detailed syntheses of complexes 1-4, Re(O)(X)(DAP) (X = Me, 1; Cl, 2; I, 3; OTf (triflate), 4) incorporating the diamido pyridine (DAP) ancillary ligand (2,6-bis((mesitylamino)methyl)pyridine) are described and shown to be effective catalysts for oxygen atom transfer (OAT) reactions of PyO to PPh(3). The catalytic activities are as follows: 4≈3 > 2 > 1. The observed electronic trend is consistent with the turnover limiting reduction of the proposed Re(VII) dioxo intermediate, Re(O)(2)(X)(DAP), during the catalytic cycle. The catalytic activity of complexes 1-3 was compared to previously published diamido amine (DAAm) oxorhenium complexes of the type Re(O)(X)(DAAm) (X = Me, 5; Cl, 6; I, 7 and DAAm = N,N-bis(2-arylaminoethyl)methylamine) which exhibit hydrolytic degradation during the catalytic reaction. Complexes 1-3 displayed higher turnover frequencies compared to 5-7. This higher catalytic activity was attributed to the more rigid DAP ligand backbone, which makes the complexes less susceptible to decomposition. However, another decomposition pathway was proposed for this catalytic system due to the observation of Re(O)(3)((MesNCH(2))(MesNCH)NC(5)H(3)) 8 in which one arm of the DAP ligand is oxidized. 相似文献
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Yoichiro Hoshina Satoru Ikegami Kyoko Fujimoto Akihiko Okuyama Tatsuhiro Harada Susan James Peter G. Griffiths Zemin Wu Michael Lilly Andrew M. Bray 《Tetrahedron letters》2005,46(52):9035-9038
2,3-Diphenylpropionic acid library for VLA-4 antagonist was synthesized on solid-phase. Comparison of the two synthetic routes via an orthogonal generation of two aromatic amino functional groups are discussed. From this work, several compounds were identified as potent VLA-4 antagonists. 相似文献
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The sample is ashed in a nickel crucible over an open flame with calcium hydroxide as the fixative; fluoride is separated by micro-diffusion and measured with a fluoride-selective electrode. The calcium hydroxide fixative permits a temperature of 800–850°C during the final ashing, so that insoluble silicates are decomposed and fluoride is converted to an acid-soluble form. Other advantages over furnace ashing at 600°C are less contamination and more rapid ashing (20 min compared to 6 h). The interference of aluminium and silica on microdiffusion was studied: perchloric acid was found to be preferable to sulphuric acid as medium. A new way for preparing calcium hydroxide suspension, low in fluoride, is described. The values found by the proposed method generally compare well with those obtained by oxygen flask combustion. Direct diffusion (i.e. without ashing) gave much lower values than the ashing methods, except for tea leaves. 相似文献
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Conservative methods for the Toda lattice equations 总被引:1,自引:0,他引:1
We are concerned with the numerical integration of the Todalattice equations by using different conservative methods. Numericalexperiments suggest that the global error for isospectral schemesdecreases exponentially with time but it is almost constantfor either symplectic or more general integrators. We providea theoretical explanation for these experimental findings. 相似文献
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Lilly J.L. Subramanian V.V. 《IEEE transactions on plasma science. IEEE Nuclear and Plasma Sciences Society》2001,29(6):927-934
Formation of an atmospheric pressure dusty air plasma is explored experimentally in this paper. The plasma is created by seeding an air flow with graphite particles and irradiating the particulates with a focused CO2 laser beam. The graphite particles are, thus, heated to thermionically emitting temperatures, and average particle temperatures and average particle number densities are measured. The presence of charges is inferred both from these measured quantities using a simple theoretical transient model, and experimentally by applying a dc bias across the irradiated region. It is found that an electron density of ~6.7 × 105 cm-3 (6.7 × 1011 m-3) can be produced at steady state in the presence of O2. This value can be increased to 3.6 × 107 cm-3 (3.6 × 1013 m -1) in the ideal case where an electron attachment to O2 is suppressed and where a lower work function particulate is used 相似文献
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