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171.
Eva Eichler Clarence Stanley Rooney Haydn Windsor Richard Williams 《Journal of heterocyclic chemistry》1976,13(4):841-844
The syntheses of some 1,8-naphthyridines substituted in the 6-position with heterocyclic groups are described. A synthetic route to 6-amino-5,7-dimethyl-1,8-naphthyridin-2(1H)one is also presented. 相似文献
172.
A SPME-HPLC-post-column fluorescent derivatization method for the direct determination of saxitoxin (STX), the most potent paralytic shellfish poisoning (PSP) toxin, in water has been developed. Commercially available SPME devices with 50 microm Carbowax templated resin (CW/TPR) coating was found to be able to pre-concentrate STX from aqueous media. A special pre-conditioning treatment of soaking the SPME coating in 0.1 M NaOH solution significantly improved the extraction efficiency. The optimal pH for the SPME process is 8.1 and the equilibration time is 40 min. The partition coefficient, K, of the distribution of STX between the SPME coating and the aqueous media was measured to be 2.99 +/- 0.04 x 10(3). Extracted toxin on the SPME stationary phase was difficult to be desorbed by the HPLC mobile phase under dynamic desorption mode. A static ion-pairing desorption technique using a desorption solvent mixture of 20 mM sodium 1-heptanesulfonate in 30% aqueous acetonitrile acidified with 50 mM sulfuric acid was developed to overcome this problem. The method detection limit and repeatability achieved by this SPME-HPLC method were 0.11 ng ml(-1) and 3.7%, respectively, with a sample volume of just 5 ml of water. This analytical method is adequate for the monitoring of the PSP toxin in fresh/drinking waters. However, serious interference was observed when this technique was applied to saline water samples. This is probably due to competition of sodium ions with the cationic STX for absorption into the SPME stationary phase. 相似文献
173.
Cy(3)PCuMe (1) undergoes reversible ligand redistribution at low temperature in solution to form the tight ion pair [Cu(PCy(3))(2)][CuMe(2)] (3). The structure of 3 was assigned on the basis of (i) the stoichiometry of the 1 = 3 equilibrium, (ii) the observation of a triplet for the PCy(3) C1 (13)C NMR resonance due to virtual coupling to two (31)P nuclei, and (iii) reverse synthesis of 1 by combining separately generated Cu(PCy(3))(2)(+) and CuMe(2)(-) ions. Complex 1 and [Cu(PCy(3))(2)][PF(6)] (5) coordinate additional PCy(3) to form (Cy(3)P)(2)CuMe and [Cu(PCy(3))(3)][PF(6)], respectively, while 3 does not. Complex 1, free PCy(3), and (bipy)(2)FeEt(2) (2) each initiate the polymerization of acrylonitrile. In each case, the polyacrylonitrile contains branches that are characteristic of an anionic polymerization mechanism. The major initiator in acrylonitrile polymerization by 1 is PCy(3), which is liberated from 1. A transient iron hydride complex is proposed to initiate acrylonitrile polymerization by 2. 相似文献
174.
Infrared fluorescence observed after exciting to ν6 (ν=1) of CD3H with a Q-switched CO2 laser yields the exponential deactivation rate constant of 0.84 ms?1 torr?1. Rate constants for deactivation of CD3H by rare gases vary from 1.4 (for He) to 0.029 (for Xe) ms?1 torr?1. 相似文献
175.
176.
Hixson KK Rodriguez N Camp DG Strittmatter EF Lipton MS Smith RD 《Electrophoresis》2002,23(18):3224-3232
A method for the complete peptide mapping of the model integral membrane protein bacteri-orhodopsin is demonstrated. Utilizing more effective enzymatic digestion, procedures with capillary liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and tandem mass spectrometry (MS/MS), all predicted tryptic digestion products were detected, as well as peptides from all previously reported post-translational modifications of bacteriorhodopsin. A significant contribution of chymotryptic-like digestion products was also observed. A characterization of the behavior of hydrophobic integral membrane peptides in a reversed-phase liquid chromatographic separation is also provided. The method reported here offers improved compatibility of the solubilizing reagents with both the chromatography and mass spectrometry, rendering it suitable for high-throughput proteomic applications. 相似文献
177.
Eric J.L. McInnes Grigore A. Timco Richard E.P. Winpenny 《Coordination chemistry reviews》2005,249(23):2577-2590
Studies of two distinct classes of chromium(III) cage complexes are discussed. The first are compact oxo- and carboxylate cages, made by heating precursors to high temperature under a flow of nitrogen. One of these cages, [Cr12O9(OH)3(O2CCMe3)15], has an S = 6 spin ground state which proves a very interesting subject for study by EPR and MCD spectroscopy. Use of other carboxylates leads to other octa- and dodeca-nuclear complexes. The second class of compounds are homo- and hetero-metallic wheels and chains bridged by fluoride and carboxylates. These include the first heterometallic anti-ferromagnetically coupled ring systems and are being widely studied in areas as diverse as magnetic cooling and quantum information processing. The mechanism by which these unusual cyclic and acyclic structures form is discussed. 相似文献
178.
Drummy LF Koerner H Farmer K Tan A Farmer BL Vaia RA 《The journal of physical chemistry. B》2005,109(38):17868-17878
With the use of high-resolution transmission electron microscopy the structure and morphology of montmorillonite (MMT), a material of current interest for use in polymer nanocomposites, was characterized. Using both imaging theory and experiment, the procedures needed to generate lattice images from MMT were established. These procedures involve careful control of the microscope's objective lens defocus to maximize contrast from features of a certain size, as well as limiting the total dose of electrons received by the sample. Direct images of the MMT lattice were obtained from neat Na+ MMT, organically modified MMT, and organically modified MMT/epoxy nanocomposites. The degree of crystallinity and turbostratic disorder were characterized using electron diffraction and high-resolution electron microscopy (HREM). Also, the extent of the MMT sheets to bend when processed into an epoxy matrix was directly visualized. A minimum radius of curvature tolerable for a single MMT sheet during bending deformation was estimated to be 15 nm, and from this value a critical failure strain of 0.033 was calculated. HREM can be used to improve the understanding of the structure of polymer nanocomposites at the nanometer-length scale. 相似文献
179.
Synthesis of some dibenzodiazepinone derivatives as potent and m2-selective antimuscarinic compounds
Victor I. Cohen Biyun Jin Miriam S. Gitler Rosanna A. La De Cruz Waclaw J. Rzeszotarski Barry R. Zeeberg Jesse Baumgold Richard C. Reba 《Journal of heterocyclic chemistry》1994,31(4):787-791
Two series of 5-[[4-[4-(dialkylamino)butyl]-l-cyclohexyl]acetyl], and 5-[(dialkylamino)acyl]-10,11-dihydro-5H- dibenzo[b,e][1,4]diazepin-11-ones were synthesized as potential m2-selective ligands 1,2. Their affinity and selectivity for the muscarinic cholinergic receptor m-AChR subtypes were determined. Replacing a nitrogen with CH in the piperidine ring of 5-[[4-[4-(dialkylamino)butyl]-l-piperidinyl]acetyl]-10,11-dihydro-5H-dibenzo-[b,e][1,4]diazepin-11-ones 3 significantly altered the affinity and selectivity to the muscarinic receptor subtypes. 相似文献
180.
Richard H. Jones Christopher A. Ramsden Helen L. Rose 《Journal of heterocyclic chemistry》1996,33(4):1031-1034
Irradiation of 2-phenylbenzimidazole ( 3 ) in the presence of methyl acrylate (20 equivalents) using a medium pressure mercury lamp gives methyl 2-(2-phenylbenzimidazol-1-yl)propionate ( 4 ) (75%) whose structure has been confirmed by an X-ray analysis. A similar reaction using acrylonitrile gave only a low yield (1%) of the corresponding propionitrile derivative 5 . A mechanism involving photoexcitation of 2-phenylbenzimidazole ( 3 ) followed by sequential single electron transfer, proton transfer and radical coupling is proposed to account for the formation of the novel photoadducts 4 and 5 . 相似文献