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171.
172.
    
A selective and sensitive method for the determination of europium was developed. Other lanthanides and oxidants do not require separation. The method is based on the redox reaction of Eu(III) with 2,2-biquinoxalyl. It was checked for the range of 0.5 to 10 g/Eu/mL. Sm(III) does not interfere in 1000-fold excess.Dedicated to Professor Dr. Dieter Klockow on the occasion of his 60th birthday  相似文献   
173.
A sensitive and specific liquid chromatography electrospray ionisation-tandem mass spectrometry method for determination of new non-imidazole histamine H(3) receptor antagonist 1-[3-(4-tert-butylphenoxy)propyl]piperidine (DL76) in rat serum has been developed and validated. Chromatography was performed on a XBridge? C18 analytical column (2.1?×?30?mm, 3.5?μm, Waters, Ireland) with gradient elution using a mobile phase containing acetonitrile and water with an addition of 0.1% of formic acid. Detection was achieved by an Applied Biosystems MDS Sciex (Concord, Ontario, Canada) API 2000 triple quadrupole mass spectrometer. Electrospray ionization (ESI) was used for ion production. The limit of detection in the SRM mode was found to be 0.5?ng?mL(-1). The limit of quantification was 1?ng?mL(-1). The precision and accuracy for both intra- and inter-day determination of DL76 ranged from 1.65 to 15.09% and from 88.74 to 113.43%. The results of this analytical method validation allow to carry out pharmacokinetic studies in rats. The method was used for the pilot study of the pharmacokinetic behavior of DL76 in rats after intravenous administration.  相似文献   
174.
The two title mononuclear compounds are four‐coordinate bis[N‐(5‐oxo‐4,4‐diphenyl‐4,5‐dihydro‐1H‐imidazolidin‐2‐ylidene)glycinato]copper(II) dimethylformamide disolvate, [Cu(C17H14N3O3)2]·2C3H7NO, (I), and five‐coordinate aquabis[N‐(5‐oxo‐4,4‐diphenyl‐4,5‐dihydro‐1H‐imidazolidin‐2‐ylidene)glycinato]copper(II) dimethylformamide disolvate, [Cu(C17H14N3O3)2(H2O)]·2C3H7NO, (II). In (I), the CuII ion lies on an inversion centre with one‐half of the complex molecule in the asymmetric unit, while in (II) there are two independent ligand molecules in the asymmetric unit, with the CuII ion and coordinated water molecule located on a general position. In both crystal structures, the complex molecules assemble in ribbons via N—H...O hydrogen‐bond networks.  相似文献   
175.
Solution equilibrium studies on the Cu(II)–polyamine–histidine ternary systems (polyamine: ethylenediamine (en), diethylenetriamine (dien), N,N,N′,N″,N″-pentamethyldiethylenetriamine (Me5dien)) have been performed by pH-potentiometry, UV–Vis spectrophotometry and EPR methods. The obtained results suggest the formation of the mixed-ligand complexes with [Cu(A)(His)]+ stoichiometry in all studied systems. Additionally, in the systems with dien and Me5dien protonated [Cu(A)(H–His)]2+ species also exists in acid solution. Our spectroscopic results indicate the tetragonal geometry for the [Cu(en)(His)]+, the geometry slightly deviated from square pyramidal for the [Cu(dien)(His)]+ and strongly deviated from square pyramidal towards trigonal bipyramidal for the [Cu(Me5dien)(His)]+ species. The coordination modes in these mixed-ligand complexes are discussed.  相似文献   
176.
The crystal and molecular structure of a polymeric Cu(II)-orotate complex, [Cu(μ-HOr)(H2O)2]n, has been reinvestigated by single crystal X-ray diffraction. It is shown that several synergistic interactions: two axial Cu-O interactions; intramolecular and intermolecular hydrogen bonds; and π-π stacking between the uracil rings contribute to the stability of the crystal structure. The Raman and FT-IR spectra of the title complex are reported for the first time. Comprehensive theoretical studies have been performed by using three unrestricted DFT methods: B3LYP; and the recently developed M06, and M05-2X density functionals. Clear-cut assignments of all the bands in the vibrational spectra have been made on the basis of the calculated potential energy distribution, PED. The very strong Raman band at 1219 cm−1 is diagnostic for the N1-deprotonation of the uracil ring and formation of the copper-nitrogen bond, in this complex. The Cu-O (carboxylate) stretching vibration is observed at 287 cm−1 in the IR spectrum, while the Cu-N (U ring) stretching vibration is assigned to the strong Raman band at 263 cm−1. The molecular structure and vibrational spectra (frequencies and intensities) calculated by the M06 functional method are very similar to the results obtained by the B3LYP method, but M06 performs better than B3LYP in calculations of the geometrical parameters and vibrational frequencies of the interligand O-H?O hydrogen bonding. Unfortunately, the M05-2X method seriously overestimates the strength of interligand hydrogen bond.  相似文献   
177.
Reactions of R2P-P(SiMe3)Li with [Cp2MCl2] (M = Zr, Hf) in hydrocarbons yield the related terminal phosphanylphosphido complexes [Cp2M(Cl){(Me3Si)P-PR2P1}] (R = iPr and tBu). The solid state structures of [Cp2M(Cl){P(SiMe3)-PiPr2P1}] (M = Zr, Hf) were established by single crystal X-ray diffraction studies. The phosphido-P atoms adopt almost planar geometries and the phosphanyl P atoms adopt pyramidal geometries. The reaction of a mixture of (Me3Si)2PLi and Ph2P-P(SiMe3)Li with [CpZrCl3] in toluene yields the dinuclear complex [Cp2Zr2Cl5(Ph2PPPSiMe3)(Li THF DME)].  相似文献   
178.
Although the influence of structurally modified sterols on artificial membranes has been intensively investigated, studies on the properties of stanols, which are saturated analogs of sterols, are very rare. Therefore, we have performed Grazing Incidence X-ray Diffraction (GIXD) experiments aimed at studying in-plane organization of a plant stanol-β-sitostanol monolayer and its mixtures with 1,2-dipalmitoyl-sn-glycero-3-phosphocholine - DPPC at the air/water interface. The collected GIXD data, resulting in-plane parameters and BAM images provide information on molecular organization and in-plane ordering of the investigated films. It was found that the lateral organization of β-sitostanol/DPPC monolayers depends on their composition. The oblique structure of the in-plane lattice of tilted hydrophobic region of molecules, found for DPPC film, is maintained at 10 mol% of stanol in the system. However, at 30 and 90 mol% of stanol in the mixture, the arrangement of molecules is hexagonal and they are oriented perpendicularly to the interface. With the addition of stanol the extend of the in-plane order of the monolayers decreases. Moreover, in mixtures the ordered domains consist of both monolayer's components. Additionally, β-sitostanol film is of similar in-plane organization as the corresponding sterol monolayer (β-sitosterol) and stanol induces condensing effect on DPPC.  相似文献   
179.
A new and unusual synthesis of benzothiazine‐fused pyrrolo[3,4‐c]coumarins, involving the ring‐opening of coumarin‐based dihydrobenzothiazoles and subsequent [4+1] cycloaddition reaction with isocyanides, was described. Thus, simple heating of various 3‐(2,3‐dihydro‐2‐methylbenzo[d]thiazol‐2‐yl)coumarins with isocyanides produced the title compounds in good yields under solvent‐free conditions.  相似文献   
180.
Novel α‐(acyloxy)‐α‐(quinolin‐4‐yl)acetamides were synthesized by the Passerini three‐component reaction between an isocyanide, quinoline‐4‐carbaldehyde, and arenecarboxylic acids in H2O. The reactions were carried out in one pot at room temperature with quantitative yields.  相似文献   
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