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101.
[reaction: see text] The use of N-alkoxyacrylamides as substrates for Lewis acid catalyzed Diels-Alder reactions has been examined. Enantioselectivities up to 92% ee have been achieved using very simple chiral Lewis acids prepared from triisobutylaluminum and 2,2-dimethyl-alpha,alpha,alpha',alpha'-tetra-1-naphthalenyl-TADDOL (1-NaphtTADDOL). The use of Yamamoto's Zn-BINOL, easily prepared from Et2Zn and 1,1'-bi-2-naphthol (BINOL), proved to be even more efficient, and enantioselectivities up to 96% ee were achieved. 相似文献
102.
A computer program is described for the rapid calculation of solution and polycrystalline electron spin resonance spectra of systems containing one unpaired electron. The calculation time is virtually independent of the number of e.s.r. transitions considered, e.g., morphamquat radical cation (3025 lines) requires 4.5 s. Second-order corrections and line-width anisotropy can be included in the simulation. The graphical output may be matched to the output of any e.s.r. spectrometer. Instrumental parameters, e.g. modulation amplitude and time constant, are accounted for in the calculation of the simulated spectrum which enables exact comparison between experimental and simulated spectra. To accommodate mixtures of paramagnetic species, a spectrum addition facility is provided; the output may be presented as an absorption or as any derivative. Spectra originating from isotopically substituted molecules may be calculated routinely and quickly, without the necessity for prior calculation of the relative contributions of the various combinations of isotopic nuclei.Several examples are given, illustrating the usefulness of this program in extracting spectral information under most experimental conditions. 相似文献
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Ivana Tatárová René Fáber Renaud Denoyel Milan Polakovič 《Journal of chromatography. A》2009,1216(6):941-947
The quantitative characterization of pore structure of Sartobind Q, a strongly basic membrane anion exchanger that is formed by cross-linked cellulose support and a hydrogel layer on its pore surface, was made combining the results obtained by several experimental techniques: liquid impregnation, batch size-exclusion, inverse size-exclusion chromatography, and permeability. Mercury intrusion and nitrogen sorption porosimetry were carried out for a dry cellulose support membrane in order to get additional information for building a model of the bimodal pore structure. The model incorporated the distribution of the total pore volume between transport and gel-layer pores and the partitioning of solutes of different molecular weights was expressed through the cylindrical pore model for the transport pores and random plane model for the gel layer. The effect of composition of liquid phase on the pore structure was investigated in redistilled water, phosphate and Tris–HCl buffers containing up to 1 M NaCl. Evident differences in the bimodal pore structure were observed here when both the specific volume and size of the hydrogel layer pores significantly decreased with the ionic strength of liquid phase. 相似文献
109.
Renaud Lavalley Gustav Amberg Henrik Alfredsson 《European Journal of Mechanics - B/Fluids》2001,20(6):771
The present work investigates thermocapillary flow in a cylindrical configuration using large Prandtl number liquids. The flow is studied using coordinated simulations and experimental optical methods such as PIV and flow visualization. In this way, properties of the oscillatory state can be obtained in great detail. Considerable attention is given to the search for the parameters influencing the onset of the instability. It is found that the onset of oscillations can be correlated using a thermocapillary Reynolds number. The oscillations take the form of a standing wave close to the onset, which is replaced by a travelling wave for stronger forcing. The selection of azimuthal wave number of the oscillatory mode is determined from geometrical parameters, and resembles the wave number selection in vortex ring instabilities. Throughout we obtain good agreement between experiments and simulations using a mathematical model with an undeformed adiabatic free surface. 相似文献
110.
Robert J. Messinger Tan Vu Huynh Renaud Bouchet Vincent Sarou-Kanian Michaël Deschamps 《Magnetic resonance in chemistry : MRC》2020,58(11):1118-1129
Magic-angle-spinning (MAS) enhances sensitivity and resolution in solid-state nuclear magnetic resonance (NMR) measurements. MAS is obtained by aerodynamic levitation and drive of a rotor, which results in large centrifugal forces that may affect the physical state of soft materials, such as polymers, and subsequent solid-state NMR measurements. Here, we investigate the effects of MAS on the solid-state NMR measurements of a polymer electrolyte for lithium-ion battery applications, poly(ethylene oxide) (PEO) doped with the lithium salt LiTFSI. We show that MAS induces local chain ordering, which manifests itself as characteristic lineshapes with doublet-like splittings in subsequent solid-state 1 H, 7 Li, and 19 F static NMR spectra characterizing the PEO chains and solvated ions. MAS results in distributions of stresses and hence local chain orientations within the rotor, yielding distributions in the local magnetic susceptibility tensor that give rise to the observed NMR anisotropy and lineshapes. The effects of MAS were investigated on solid-state 7 Li and 19 F pulsed-field-gradient (PFG) diffusion and 7Li longitudinal relaxation NMR measurements. Activation energies for ion diffusion were affected modestly by MAS. 7Li longitudinal relaxation rates, which are sensitive to lithium-ion dynamics in the nanosecond regime, were essentially unchanged by MAS. We recommend that NMR researchers studying soft polymeric materials use only the spin rates necessary to achieve the desired enhancements in sensitivity and resolution, as well as acquire static NMR spectra after MAS experiments to reveal any signs of stress-induced local ordering. 相似文献