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M A Alliegro K D Dyer E J Cragoe B M Glaser M C Alliegro 《Journal of chromatography. A》1992,582(1-2):217-223
An assay for amiloride was devised for efficient use with the wide variety of analogues available. Amiloride was extracted from 1-ml plasma samples by elution from a C8 preparative column with 6% acetonitrile-45% methanol-5.4% acetic acid, adjusted to pH 4.0 with trimethylamine. Samples were lyophilized, resuspended in 50% methanol, filtered through 0.22-microns Spin-X cartridges, applied to a reversed-phase C18 column, and eluted in a 0-50% acetonitrile gradient in 0.4% acetic acid, pH 4.5 (1.2 ml/min). Detection by ultraviolet absorbance at 360 nm was linear from 1 to 1000 ng. Versatility of the method was demonstrated with the analogues benzamil, 6-hydro-, 6-iodo-, 5-hexamethylene-, and 5-chlorobenzyl-2',4'-dimethylbenzyl-amiloride. 相似文献
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A facile synthesis of 2-formyl-1,8-naphthalenediol is reported. Its potential as a general precursor for the preparation of unsymmetrical multidentate chelating ligand systems based on 1,8-naphthalenediol is demonstrated by the synthesis of the dinucleating ligand L(4-)(H(4)L=N,N'-bis(2-(1,8-naphthalenediol)methylidene)propylenediamine). Reaction of H(4) L with copper acetate results in the formation of the unsymmetrical dinuclear Cu(II) complex [LCu(2)](3), which has been structurally characterized by single-crystal X-ray diffraction. One Cu(II) ion is coordinated by a N(2)O(2) compartment of L(4-) and the other Cu(II) ion is coordinated by an O(4) compartment of L(4-) while they are bridged by two aryloxide functions of L(4-). A dimerization of two molecules of 3 to a tetranuclear entity 3(2) occurs through formation of weak apical Cu--O interactions. Analysis of the temperature dependent magnetic susceptibility measurements (2--290 K) established a strong intradimer exchange coupling J(12)=-371 cm(-1). This strong superexchange interaction fits nicely in a magneto-structural correlation which has been established for dinuclear bis(phenoxide)-bridged Cu(II) complexes demonstrating the electronic equivalence of the aryloxides of a phenol and 1,8-naphthalenediol. 相似文献
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Robert Glaser Menachem Twaik Shimona Geresh Jeanine Blumenfeld 《Tetrahedron letters》1977,18(52):4635-4638
Z--acetamidocinnamic acid was hydrogenated with neutral diphosphine-rhodium(I) complexes containing trans-1,2-bis(diphenylphosphinomethyl) cycloalkanes to give N-acetylphenylalanine: 86 % e.e.-(R) [(1R,2R)-cyclobutane]; 63 % e.e.-(R) [(1R,2R)-cyclopentane]; 35 % e.e.-(S) [(1S,2S)-cyclohexane]; and 82 % e.e.-(R) [(2R,3R)-DIOP]. Similarly, -acetamidoacrylic acid was hydrogenated to give N-acetylalanine: 72 % e.e.-(R) [(1R,2R)-cyclobutane]; 72 % e.e.-(R) [(1R,2R)-cyclopentane]; 40 % e.e.-(S) [(1S,2S)-cyclohexane]; and 73 % e.e.-(R) [(2R,3R)-DIOP]. 相似文献
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Guibin Ma Andreas Fischer Julius Glaser 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(3):m177-m178
The title compound, bis(dimethyl sulfoxide)triiodothallium(III), [TlI3(C2H6OS)2], was crystallized from equimolar amounts of TlII and I2 in a dimethyl sulfoxide (DMSO) solution. After the initial redox reaction, the thallium(III)–iodo complex forms and precipitates as a DMSO solvate. In the crystal structure, Tl is surrounded by three iodide ligands in the equatorial plane and two O‐coordinated DMSO molecules in the axial positions, forming a slightly distorted trigonal bipyramid. The complex lies on a twofold rotation axis, making the DMSO molecules and two of the I atoms crystallographically equivalent. 相似文献
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Vosegaard T Kehlet C Khaneja N Glaser SJ Nielsen NC 《Journal of the American Chemical Society》2005,127(40):13768-13769
We have investigated the use of optimal control theory for the design of improved multiple-quantum excitation schemes for the popular multiple-quantum magic-angle spinning NMR experiment for quadrupolar nuclei with half-integer quadrupolar spin. The advantage of the new low-power experiments, termed OCFASTER, is demonstrated by sensitivity improvements approaching 50% for 87Rb in RbClO4 and RbNO3 as compared to FASTER and standard strong-pulse excitation schemes. 相似文献