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991.
Tomoko Kemmei Shuji Kodama Hironori Fujishima Atsushi Yamamoto Yoshinori Inoue Kazuichi Hayakawa 《Analytica chimica acta》2012
The chelating agent EDTA is widely used, and as a result is showing up widely in the aquatic environment. Here we describe a preconcentration procedure for measuring EDTA concentration in sea water samples by HPLC. The procedure consists of forming an Fe(III) complex followed by solid-phase extraction using an activated carbon cartridge. After the preconcentration, EDTA was quantified by HPLC with ultraviolet detection (260 nm). The enrichment permitted the determination of EDTA at concentrations as low as 1 nM. Good recoveries were obtained for both brackish and full-strength sea water with high repeatability (RSD < 6%). The method was applied to sea water samples taken from near the mouth of the Oyabe River in Japan. 相似文献
992.
Shin-ichi Takekuma Manami Yamamoto Aki Nakagawa Tomohiro Iwata Toshie Minematsu Hideko Takekuma 《Tetrahedron》2012,68(39):8318-8329
Wittig reaction of (E)-3-(3-guaiazulenyl)propenal (11) with (3-guaiazulenylmethyl)triphenylphosphonium bromide (9) in ethanol containing NaOEt at 25 °C for 24 h under argon gives the title new (2E,4E)-1,3-butadiene derivative 4, in 33% isolated yield, which upon treatment with hexafluorophosphoric acid (i.e., 65% HPF6 aqueous solution) in tetrahydrofuran (=THF) at 25 °C for 1 h under aerobic conditions affords a new air (two-electron) oxidation product (E)-ethylene-1,2-bis(3-guaiazulenylmethylium) bis(hexafluorophosphate) (14), quantitatively, and further, zinc-reduction of 14 in trifluoroacetic acid (=CF3COOH) at 0 °C for 1 h under argon reverts 4, quantitatively. Along with the above interesting results, our discovered another preparation method, spectroscopic properties, crystal structure, and electrochemical behavior of 4, which serves as a strong two-electron donor and acceptor, compared with those of the previously reported (E)-1,2-di(3-guaiazulenyl)ethylene (3) are documented in detail. 相似文献
993.
An efficient synthetic method for the formation of 2,3-dihydro-1H-inden-1-one derivatives through a Ni-catalyzed intramolecular hydroacylation of 2-(prop-2-ynyl)benzaldehydes has been developed. Examination of various nickel and other transition metal catalysts and phosphine ligands showed that the use of Ni(COD)2 catalyst combined with P(i-Pr)3 ligand was the best choice to the success of the present intramolecular hydroacylation. A wide range of functional groups were tolerated, affording the corresponding substituted α-lidene-2,3-dihydro-1H-inden-1-ones in good to high yields with a sole E-selectivity under present reaction conditions. 相似文献
994.
Giovanni Ferrara Tienan Jin Md. Akhtaruzzaman Ashraful Islam Liyuan Han Hua Jiang Yoshinori Yamamoto 《Tetrahedron letters》2012,53(15):1946-1950
A facile, efficient, and general synthetic method for iodo-substituted benzo[b]naphtho[2,1-d]thiophenes has been developed via a cascade cyclization of thioanisole-substituted aryldiynes using iodine. A new donor–π linker–acceptor (D–π–A) organic dye, G1, with the benzo[b]naphtho[2,1-d]thiophene moiety as an electron donor has been synthesized, and the performance of dye-sensitized solar cell based on G1 has been investigated. 相似文献
995.
Arichi N Inase A Eto S Mizukoshi T Yamamoto J Iwai S 《Organic & biomolecular chemistry》2012,10(11):2318-2325
The (6-4) photoproduct is one of the major damaged bases produced by ultraviolet light in DNA. This lesion is known to be alkali-labile, and strand breaks occur at its sites when UV-irradiated DNA is treated with hot alkali. We have analyzed the product obtained by the alkali treatment of a dinucleoside monophosphate containing the (6-4) photoproduct, by HPLC, NMR spectroscopy, and mass spectrometry. We previously found that the N3-C4 bond of the 5' component was hydrolyzed by a mild alkali treatment, and the present study revealed that the following reaction was the hydrolysis of the glycosidic bond at the 3' component. The sugar moiety of this component was lost, even when a 3'-flanking nucleotide was not present. Glycosidic bond hydrolysis was also observed for a dimer and a trimer containing 5-methyl-2-pyrimidinone, which was used as an analog of the 3' component of the (6-4) photoproduct, and its mechanism was elucidated. Finally, the alkali treatment of a tetramer, d(GT(6-4)TC), yielded 2'-deoxycytidine 5'-monophosphate, while 2'-deoxyguanosine 3'-monophosphate was not detected. This result demonstrated the hydrolysis of the glycosidic bond at the 3' component of the (6-4) photoproduct and the subsequent strand break by β-elimination. It was also shown that the glycosidic bond at the 3' component of the Dewar valence isomer was more alkali-labile than that of the (6-4) photoproduct. 相似文献
996.
Murai M Okuzono T Yamamoto M Toyotama A Yamanaka J 《Journal of colloid and interface science》2012,370(1):39-45
We examine the compression of charged colloidal crystals under the influence of gravitational force by monitoring the spatiotemporal variations of Bragg diffraction from the crystal lattice. We use the dilute aqueous dispersions of colloidal silica particles (diameter=216 nm, charge number=733, a particle volume fraction φ=0.06) in the presence of 5-15 μM sodium chloride. The sedimentation profiles of the colloidal crystals along the crystal height are determined by in situ fiber optics reflection spectroscopy. The time evolutions of the sedimentation profiles are calculated by numerical simulations based on a phenomenological continuum model that explicitly incorporates the electrostatic interparticle interactions. The simulation results correctly describe the experiments at sufficiently high ionic strength. 相似文献
997.
trans-Cyclooctanediyl-bridged [OSSO]-type ligand 4 reacts with TiCl(4)(thf)(2) in toluene to produce the corresponding titanium(IV) dichloro complexes as an inseparable mixture of cis-α isomer 6a and cis-β isomer 6b in a ratio of 2:1, whereas treatment of dilithio salt of 4 with TiCl(3)(thf)(3) in Et(2)O afforded chloride-bridged dimeric titanium(III) complex 8, which indicated the antiferromagnetic character in a nonpolar solvent solution. Di(isopropoxy) titanium(IV) complex 10 having a C(2)-symmetric cis-α configuration was synthesized by the reaction of 4 with Ti(O(i)Pr)(4) in toluene as yellow crystals. Moreover, the reaction of 4 with Ti(NEt(2))(4) in toluene resulted in the unexpected formation of [OSSO]-type bis(phenolato)-bridged dinuclear diamido titanium(IV) complex 11, which adopted a distorted tetrahedral geometry on the titanium center. These titanium complexes were characterized on the basis of their NMR spectroscopic data, and the molecular structures of complexes 8, 10, and 11 were established by single crystal X-ray diffraction. The titanium(IV) and (III) complexes 6 and 8 upon activation with a cocatalyst in toluene polymerized 1-hexene isospecifically to produce poly(1-hexene) having high molecular weight (M(w) = 22,000-52,000 g mol(-1)) and relatively narrow polydispersity (M(w)/M(n) = 1.7-1.8), albeit with low activity [0.27-1.0 g mmol(cat)(-1) h(-1)]. 相似文献
998.
5-O-(4-[125 I]Iodobenzyl)-L-ascorbic acid: electrophilic radioiodination and biodistribution in mice
Kim J Kino T Kato H Yamamoto F Sano K Mukai T Maeda M 《Chemical & pharmaceutical bulletin》2012,60(2):235-240
As a part of our efforts to develop potential imaging agents for ascorbate bioactivity, 5-O-(4-[(125)I]iodobenzyl)-L-ascorbic acid ([(125)I]1) was prepared through a two-step sequence which involved radioiodo-destannylation of a protected tributylstannyl precursor 6, followed by hydrolysis in acidic methanol of the protecting groups in 61% overall radiochemical yield, with a radiochemical purity of over 98% and a specific activity of more than 15.4?GBq/μmol. Tissue distribution of [(125)I]1 in tumor-bearing mice showed signs of distribution profiles similar to the reported results for 6-deoxy-6-[(18)F]fluoro-L-ascorbic (6-(18)FAsA) acid and 6-deoxy-6-[(131)I]iodo-L-ascorbic acid (6-(131)IAsA) but with notable differences in the adrenal glands, in which considerably lower uptake of radioactivity and rapid clearance with time were observed. Pretreatment of mice with a known inhibitor of ascorbate transport, sulfinpyrazone, did not produce any significant change in the adrenal uptake of radioactivity after injection of [(125)I]1 compared to the control, suggesting that uptake in the adrenal glands is independent of the sodium-dependent vitamin C transporter 2 transport mechanism. Introduction of a bulky substituent at C-5 on AsA, such as an iodobenzyloxy group, may not be suitable for the design of analogs that may still be able to maintain characteristic distribution properties in vivo seen with AsA itself. 相似文献
999.
Atsuyoshi Nakayama Minoru UkitaJun Iyoda Norioki KawasakiNoboru Yamamoto 《Polymer Degradation and Stability》2012,97(1):14-20
Copolyesters of poly(ε-caprolactone) diol and 1,18-octadecane dicarboxylic acid were synthesized by polyaddition. The copolymers have a "mixed" structure of ’polyester-polyethylene’. Characterization was carried out by using 1H and 13C NMR, FT-IR, viscosities, DSC, and GPC. The tensile strength varied from 11.9 to 19.9 MPa, and elongation at break varied from 370 to 660 %, respectively. Biodegradability was evaluated by enzymatic hydrolysis (lipases from Rhizopus arrhizus and Candida cylindracea and an esterase form hog liver) and by soil burial test. Both tests showed that the copolyesters were characterized by enhanced biodegradability. 相似文献