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941.
Lumbierres M Palomo JM Kragol G Roehrs S Müller O Waldmann H 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(24):7405-7415
A new flexible and efficient methodology for the solid-phase synthesis of lipidated peptides has been developed. The approach is based on the use of previously synthesized building blocks and overcomes the limitations of previously reported methods, since long doubly lipidated peptides can be synthesized by using this route. Furthermore, it was thus possible to prepare a large number of N- and H-Ras peptides bearing a wide range of reporter and/or linking groups--efficient tools for the investigation of biological processes. In terms of efficiency and flexibility this solid-phase method is superior to the solution-phase synthesis. It gives pure peptides in multimilligram amounts within a much shorter time and with superior overall yield. 相似文献
942.
The electrochemical reduction of antifouling agent 2-thiocyanomethylthiobenzothiazole (TCMTB) was investigated by cyclic and pulse differential voltammetry. The irreversible electrode reduction of TCMTB proceeded by ECEC reaction mechanism by two electrons transfer with one irreversible wave. Upon the basis of electrochemical evidence, the electrodic reaction mechanism was suggested to formation of mercaptobenzothiazole (MTB) in solution.Subsequently, a pulse differential method is described for the formation of TCMTB based on this electroreduction. Having been obtained a detection limit of 1.0 × 10−7 mol L−1 and recovery to 98% to concentration of 2.0 × 10−6 mol L−1. Therefore, the proposed method in this study is practical, sensitive and accurate for the analysis of TCMTB in tannery wastewater samples. 相似文献
943.
Takakazu Yamamoto Abla Mahmut Masahiro Abe Shin‐Ichi Kuroda Tatsuya Imase Shintaro Sasaki 《Journal of Polymer Science.Polymer Physics》2005,43(16):2219-2224
An alternating copolymer, Copoly‐1 , of thiophene and N‐(phenylethynyl)pyrrole was prepared by palladium‐catalyzed polycondensation. Powder X‐ray diffraction (XRD) analysis indicated that Copoly‐1 formed a stacked packing structure with doubly‐running polymer main chains. Optical data support the molecular and packing structures of Copoly‐1 . © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 2219–2224, 2005 相似文献
944.
Calderoni F Demartin F Iapalucci MC Laschi F Longoni G Zanello P 《Inorganic chemistry》1996,35(4):898-905
A reinvestigation of the redox behavior of the [Fe(3)(&mgr;(3)-S)(CO)(9)](2)(-) dianion led to the isolation and characterization of the new [Fe(5)S(2)(CO)(14)](2)(-), as well as the known [Fe(6)S(6)(CO)(12)](2)(-) dianion. As a corollary, new syntheses of the [Fe(3)S(CO)(9)](2)(-) dianion are also reported. The [Fe(5)S(2)(CO)(14)](2)(-) dianion has been obtained by oxidative condensation of [Fe(3)S(CO)(9)](2)(-) induced by tropylium and Ag(I) salts or SCl(2), or more straightforwardly through the reaction of [Fe(4)(CO)(13)](2)(-) with SCl(2). The [Fe(6)S(6)(CO)(12)](2)(-) dianion has been isolated as a byproduct of the synthesis of [Fe(3)S(CO)(9)](2)(-) and [Fe(5)S(2)(CO)(14)](2)(-) or by reaction of [Fe(4)(CO)(13)](2)(-) with elemental sulfur. The structures of [N(PPh(3))(2)](2)[Fe(5)S(2)(CO)(14)] and [N(PPh(3))(2)](2)[Fe(6)S(6)(CO)(12)] were determined by single-crystal X-ray diffraction analyses. Crystal data: for [N(PPh(3))(2)](2)[Fe(5)S(2)(CO)(14)], monoclinic, space group P2(1)/c (No. 14), a = 24.060(5), b = 14.355(6), c = 23.898(13) ?, beta = 90.42(3) degrees, Z = 4; for [N(PPh(3))(2)](2)[Fe(6)S(6)(CO)(12)], monoclinic, space group C2/c (No. 15), a = 34.424(4), b = 14.081(2), c = 19.674(2) ?, beta = 115.72(1) degrees, Z = 4. The new [Fe(5)S(2)(CO)(14)](2)(-) dianion shows a "bow tie" arrangement of the five metal atoms. The two Fe(3) triangles sharing the central Fe atom are not coplanar and show a dihedral angle of 55.08(3) degrees. Each Fe(3) moiety is capped by a triply bridging sulfide ligand. The 14 carbonyl groups are all terminal; two are bonded to the unique central atom and three to each peripheral iron atom. Protonation of the [Fe(5)S(2)(CO)(14)](2)(-) dianion gives reversibly rise to the corresponding [HFe(5)S(2)(CO)(14)](-) monohydride derivative, which shows an (1)H-NMR signal at delta -21.7 ppm. Its further protonation results in decomposition to mixtures of Fe(2)S(2)(CO)(6) and Fe(3)S(2)(CO)(9), rather than formation of the expected H(2)Fe(5)S(2)(CO)(14) dihydride. Exhaustive reduction of [Fe(5)S(2)(CO)(14)](2)(-) with sodium diphenyl ketyl progressively leads to fragmentation into [Fe(3)S(CO)(9)](2)(-) and [Fe(CO)(4)](2)(-), whereas electrochemical, as well as chemical oxidation with silver or tropylium tetrafluoroborate, in dichloromethane, generates the corresponding [Fe(5)S(2)(CO)(14)](-) radical anion which exhibits an ESR signal at g = 2.067 at 200 K. The electrochemical studies also indicated the existence of a subsequent one-electron anodic oxidation which possesses features of chemical reversibility in dichloromethane but not in acetonitrile solution. A reexamination of the electrochemical behavior of the [Fe(3)S(CO)(9)](2)(-) dianion coupled with ESR monitoring enabled the spectroscopic characterization of the [Fe(3)S(CO)(9)](-) radical monoanion and demonstrated its direct involvement in the generation of the [Fe(5)S(2)(CO)(14)](n)()(-) (n = 0, 1, 2) system. 相似文献
945.
The reaction of nitric oxide with the carboxylate-bridged diiron(II) complex [Fe(2)(Et-HPTB)(O(2)CPh)](BF(4))(2) (1a) afforded the dinitrosyl adduct, [Fe(2)(NO)(2)(Et-HPTB)(O(2)CPh)](BF(4))(2) (1b), where Et-HPTB = N,N,N',N'-tetrakis(N-ethyl-2-benzimidazolylmethyl)-2-hydroxy-1,3-diaminopropane, in 69% yield. Compound 1b further reacts with dioxygen to form the bis(nitrato) complex, [Fe(2)(Et-HPTB)(NO(3))(2)(OH)](BF(4))(2) (1c). The structure of 1b was determined by X-ray crystallography (triclinic, P&onemacr;, a = 13.5765(8) ?, b = 15.4088(10) ?, c = 16.2145(10) ?, alpha = 73.656(1) degrees, beta = 73.546(1) degrees, gamma = 73.499(1) degrees, V = 3043.8(7) ?(3), T = -80 degrees C, Z = 2, and R = 0.085 and R(w) = 0.095 for 5644 independent reflections with I > 3sigma(I)). The two nitrosyl units are equivalent with an average Fe-N-O angle of 167.4 +/- 0.8 degrees. Spectroscopic characterization of solid 1b revealed an NO stretch at 1785 cm(-)(1) in the infrared and M?ssbauer parameters of delta = 0.67 mm s(-)(1) and DeltaE(Q) = 1.44 mm s(-)(1) at 4.2 K. These data are comparable to those for other {FeNO}(7) systems. An S = (3)/(2) spin state was assigned from magnetic susceptibility studies to the two individual {FeNO} centers, each of which has a nitrosyl ligand antiferromagnetically coupled to iron. A least-squares fit of the chi vs temperature plots to a theoretical model yielded an exchange coupling constant J of -23 cm(-)(1), where H = -2JS(1).S(2), indicating that the two S = (3)/(2) centers are antiferromagnetically coupled to one another. An extended Hückel calculation on a model complex, [Fe(2)(NO)(2)(NH(3))(6)(O(2)CH)(OH)](2+), revealed that the magnitudes of Fe-N-O angles are dictated by pi-bonding interactions between the Fe d(xz)() and NO pi orbitals. 相似文献
946.
Herbert Alber und Maria von Renzenberg 《Fresenius' Journal of Analytical Chemistry》1931,86(1-4):114-127
Zusammenfassung Die Beobachtung von Schlieren mit dem unbewaffneten Auge, die sogenannte visuelle Methode, erweist sich als ein Verfahren, das seinen Hauptvorteil in der ausserordentlich grossen Einfachheit besitzt. Das Fehlen jeder besonderen optischen Einrichtung ist ein so erheblicher Vorteil, dass in den meisten Fällen der Nachteil einer etwas geringeren Empfindlichkeit (n =0,0001–0,0002) aufgehoben wird, wenn er nicht sogar erwünscht ist.Überall dort, wo man rasch und ohne spezielle Hilfsmittel Schlierenbeobachtungen vornehmen will, wird die visuelle Methode geeignet sein, während das Schlierenmikroskop für die Betrachtung von sehr schwachen Schlieren und besonders für das Studium von doppeltschattierten. Schlieren vorzuziehen ist.Mittels der visuellen Methode können wir auch zahlenmäßige Angaben über die Schlierenintensität machen, also Messungen der Schlierenstärke vornehmen, wobei der Messbereich des Schlierenmikroskops bei allerdings verminderter Empfindlichkeit bis zu höheren Unterschieden in den Brechungsindices von Fliess- und Standprobe (n bis 0,0250) ergänzt wird.Die praktische Verwendbarkeit der visuellen Methode ist in vielen Parallelversuchen mit dem Schlierenmikroskop und in einigen speziellen Versuchsreihen, über welche in einer der folgenden Mitteilungen berichtet werden soll, bewiesen worden.Wir haben schon an anderer Stelle bemerkt, dass es bei der hier geübten Art des Zusammenarbeitens oft schwer ist, dem Anteil gerecht zu werden, der dem einzelnen Mitarbeiter zukommt. Die vorliegende Mitteilung setzt sich aus Material zusammen, das teilweise der Doktordissertation von Frl. Maria von Rentenberg entnommen, teilweise von Dr. H. Alber selbst gesammelt worden ist. Letzterem bin ich auch für die Arbeit dankbar, die er bei der Zusammenstellung der Abhandlung geleistet hat. 相似文献
947.
Xing‐Yun Chai Zheng‐Ren Xu Hong‐Yan Ren Hai‐Ming Shi Ya‐Nan Lu Fei‐Fei Li Peng‐Fei Tu 《Helvetica chimica acta》2007,90(11):2176-2185
Eight new benzoylated gentisyl alcohol (=2‐(hydroxymethyl)benzene‐1,4‐diol) glucosides, itosides A–H ( 1 – 8 ), together with the new pyrocatechol (=benzene‐1,2‐diol) glycoside itoside I ( 9 ) were isolated from the bark and twigs of Itoa orientalis (Flacourtiaceae). In itosides B–D ( 2 – 4 ), the gentisyl alcohol moiety was esterified by 1‐hydroxy‐6‐oxocyclohex‐2‐ene‐1‐carboxylic acid, while itosides E–H ( 5 – 8 ) contained instead an additional 2‐hydroxybenzoic acid moiety. The compounds were accompanied by the known derivatives 4‐hydroxytremulacin ( 10 ), poliothyrsoside ( 11 ), poliothyrsin ( 12 ), homaloside D ( 13 ), tremulacin, and pyrocatechol β‐D ‐glucopyranoside. The structures of the new compounds were elucidated by spectral and chemical methods. 相似文献
948.
Separation techniques coupled to inductively coupled plasma mass spectrometry (ICP-MS) is reviewed. ICP-MS technique is described briefly. Coupling of the different separation techniques are described, together with the most common applications used for each technique that has been described in the literature. An overview for the future of separation techniques coupled to ICP-MS with regard to elemental speciation is discussed. 相似文献
949.
The development of the hydration-hydrolysis processes in the 3CaOSiO2-H2O system is studied by X-ray diffraction in presence of varying contents of a new plasticizer, belonging to the lignosulphonates class. The influence of the additives upon these processes with increasing time is observed and it is shown to depend on the nature and content of the additives and the reaction time. This influence of the additives on the kinetics of the hydration-hydrolysis processes, retardation or acceleration, is due to the strong adsorption of these admixtures on the surface of the anhydrous or partially hydrated particles of the system. The influence of the additives also appears during the development of the formed hydrocompounds according to structure and composition. As a result of these complex actions provided in the forming system (3CaOSiO2-H2O), the mechanical strength is favorized mainly by certain proportions of plasticizer admixtures (0.1% LSC and 2% ADCOM). 相似文献
950.
T. Itagaki E. Rokuta H.‐S. Kuo K. Nomura T. Ishikawa B.‐L. Cho I.‐S. Hwang T. T. Tsong C. Oshima 《Surface and interface analysis : SIA》2007,39(4):299-303
We observed field emission microscopy (FEM) patterns of noble‐metal (NM) covered W nano‐tips with three different apex structures fabricated by field evaporation. Each of the three tips was terminated with a single atom, three atoms or ten atoms. We investigated the temporal changes in the FEM of these tips to discuss the stabilities in the spatial distributions of the field emission (FE) beams. The single‐atom tip showed two characteristics that were superior to the others. First, the beams emitted from the single‐atom tip were the most collimated among the three tips (the semi‐cone angle of 1.0° , FWHM). Second, adsorption of residual gas had little influence on FE from the single‐atom tip, while the other tips were easily contaminated even at ultra high vacuum, resulting in the emission fluctuation. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献