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Sammelson RE Gurusinghe CD Kurth JM Olmstead MM Kurth MJ 《The Journal of organic chemistry》2002,67(3):876-882
An efficient and selective method for the synthesis of spiro-fused (C5)-isoxazolino-(C4)-pyrazolones (C) is reported. The process consists of utilizing the Baylis-Hillman reaction-or a quicker, stepwise MAC procedure-to give I followed by 1,3-dipolar cycloaddition and Swern oxidation to give beta-ketoesters H, which were condensed with hydrazine derivatives to provide hydrazones that underwent cycloelimination. These novel spiro-fused (C5)-isoxazolino-(C4)-pyrazolones were confirmed by spectroscopic analysis as well as single-crystal X-ray of 5. We also concluded that all condensations/cycloeliminations, except with hydrazine itself, were more effective with catalysts or higher reaction temperatures. For example, TiCl(4) was an efficient catalyst for hydrazone formation and cycloelimination with methylhydrazine, while phenyl-, benzyl-, and (4-methoxyphenyl)hydrazine reacted effectively without catalyst in refluxing xylene. 相似文献
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A structural failure problem was solved using an integrated and iterative program of testing and analysis. The steps taken in solving the problem were: analytical calculations; operational testing; qualifications of analytical results; problem identification; design of corrective action; and confirmatory testing. 相似文献
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We have performed extensive small-angle neutron scattering (SANS) diffraction studies of the vortex lattice in single crystal
YNi2B2C for B‖c. High-resolution SANS, combined with a field-oscillation vortex lattice preparation technique, allows us to separate Bragg
scattered intensities from two orthogonal domains and accurately determine the unit cell angle, β. The data suggest that upon increasing field there is a finite transition width where both low- and high-field distorted
hexagonal vortex lattice phases, mutually rotated by 45°, coexist. The smooth variation of diffracted intensity from each
phase through the transition corresponds to a redistribution of populations between the two types of domains. 相似文献
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Ikhlas D. Darkhalil Joshua J. Klaassen Nick Nagels Wouter A. Herrebout Benjamin J. van der Veken Ranil M. Gurusinghe Michael J. Tubergen James R. Durig 《Journal of Raman spectroscopy : JRS》2014,45(5):392-406
Fourier transform microwave spectrum of cyclopentylamine, c–C5H9NH2 has been recorded, and seven transitions have been assigned for the most abundant conformer, and the rotational constants have been determined: A = 4909.46(5), B = 3599.01(4), and C = 2932.94(4). From the determined microwave rotational constants and ab initio MP2(full)/6‐311 + G(d,p) predicted structural values, adjusted r0 parameters are reported with distances (Å): rCα–Cβ = 1.529(3), rCβ–Cγ = 1.544(3), rCγ–Cγ = 1.550(3), rCα–N = 1.470(3), and angles (°) ∠CCN = 108.7(5), ∠CβCαCβ = 101.4(5), and τCβCαCβ′Cγ′ = 42.0(5). The infrared spectra (4000–220 cm−1) of the gas have been recorded. Additionally, the variable temperature (−60 to −100 °C) Raman spectra of the sample dissolved in liquefied xenon was recorded from (3800–50 cm−1). The four possible conformers have been identified, and their relative stabilities obtained with enthalpy difference relative to t‐Ax of 211 ± 21 cm−1 for t‐Eq ≥ 227 ± 22 cm−1 for g‐Eq ≥ 255 ± 25 cm−1 for g‐Ax. The percentage of the four conformers is estimated to be 53% for the t‐Ax, 11 ± 1% for t‐Eq, 20 ± 2% for g‐Ax and 16 ± 2% for g‐Eq at ambient temperature. The conformational stabilities have been predicted from ab initio calculations by utilizing several different basis sets up to aug‐cc‐pVTZ from both MP2(full) and density functional theory calculations by the B3LYP method. Vibrational assignments have been provided for the observed bands for all four conformers, which are predicted by MP2(full)/6‐31G(d) ab initio calculations to predict harmonic force constants, wavenumbers, infrared intensities, Raman activities, and depolarization ratios for all of the conformers. The results are discussed and compared to the corresponding properties of some related molecules. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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CD Bertram 《Contemporary Physics》2013,54(1):45-60
Collapsible tubes, which occur all over the body, have unique properties from the point of view of both physics and physiology. A brief review is attempted of first the basic observable properties, followed by simple theory to explain the steady-flow aspects and an overview of the somewhat more complex theories for unsteady flow, in particular the flow-induced oscillations. The experimental evidence from laboratory studies is reviewed with particular emphasis on the dynamical system aspects. A final section looks at the current position and prospects. 相似文献
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We have performed a series of neutron diffraction experiments from the magnetic order and the vortex lattice in single crystal
ErNi2B2C. The incommensurate magnetic structure develops additional even harmonics below the ‘ferromagnetic’ ordering temperature,
T
F of 2.3 K. This feature and the existence of rods of diffuse scattering suggest the development of ferromagnetic microdomain
walls. The magnetic structure is very sensitive to the application of a magnetic field with changes in modulation vector and
harmonic content. Studies of the vortex lattice show the presence of a 45° reorientation transition and a distorted hexagonal
to square transition as a function of applied field. Further distortions of the vortex lattice occur at T
N, but no changes are seen at T
F. 相似文献
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