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1.
Elemental I(2) and Br(2) cleanly react with the 3:3 Pt(ii) metallamacrocycle of 3,3,3',3'-tetra(n-butyl)-1,1'-terephthaloylbis(thiourea)(cis-[Pt(II)(3)(L(p)(1)-S,O)(3)]3), in chloroform at room temperature, to yield oxidative addition products; (195)Pt NMR studies reveal that a stepwise oxidative addition readily occurs to each of the Pt(ii) centres in the metallamacrocycle to yield the mixed valence species cis-[Pt(II)(2)Pt(IV)I(2)(L(p)(1)-S,O)(3)] and cis-[Pt(II)Pt(IV)(2)I(4)(L(p)(1)-S,O)(3)], and the fully oxidised cis-[Pt(IV)(3)I(6)(L(p)(1)-S,O)(3)] in solution, depending on the mole ratio I(2):3. Similar results are obtained on treatment of solutions of 3 with elemental Br(2). Treatment of the corresponding 2:2 Pt(ii) complex of 3,3,3',3'-tetraethyl-1,1'-isophthaloylbis(thiourea)(cis-[Pt(II)(2)(L(m)(1)-S,O)(2)]4) with iodine, results in facile oxidative addition to yield cis-[Pt(IV)(2)(L(m)(1)-S,O)(2)I(4)], with a trans-Pt(iv)-iodo arrangement. Molecules in the crystal structure of 5 have their trans-Pt(iv)-iodo axes essentially aligned, with very close intermolecular iodide contacts (3.775(1)A), resulting in chains of weakly bound metallamacrocycles in the solid. An alternative electrolytic synthesis method, using a simple two-compartment glass cell containing 4 and a chosen halide salt in dichloromethane, led to the formation of cis-[Pt(IV)(2)(L(m)(1)-S,O)(2)Br(4)] 6 and cis-[Pt(IV)(2)(L(m)(1)-S,O)(2)Cl(4)] 7, completing characterization of a series of first-reported trans-Pt(iv)-X (X=I, Br, Cl) metallamacrocyclic complexes. 相似文献
2.
Susan A. Bourne Katherine De Villiers Timothy J. Egan 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(2):o53-o57
The structures of three compounds with potential antimalarial activity are reported. In N,N‐diethyl‐N′‐(7‐iodoquinolin‐4‐yl)ethane‐1,2‐diamine, C15H20IN3, (I), the molecules are linked into ribbons by N—H⋯N and C—H⋯N hydrogen bonds. In N‐(7‐bromoquinolin‐4‐yl)‐N′,N′‐diethylethane‐1,2‐diamine dihydrate, C15H20BrN3·2H2O, (II), two aminoquinoline molecules and four water molecules form an R54(13) hydrogen‐bonded ring which links to its neighbours to form a T5(2) one‐dimensional infinite tape with pendant hydrogen bonds to the aminoquinolines. The phosphate salt 7‐chloro‐4‐[2‐(diethylammonio)ethylamino]quinolinium bis(dihydrogenphosphate) phosphoric acid, C15H22ClN32+·2H2PO4−·H3PO4, (III), was prepared in order to establish the protonation sites of these compounds. The phosphate ions form a two‐dimensional hydrogen‐bonded sheet, while the aminoquinoline cations are linked to the phosphates by N—H⋯O hydrogen bonds from each of their three N atoms. While the conformation of the quinoline region hardly varies between (I), (II) and (III), the amino side chain is much more flexible and adopts a significantly different conformation in each case. Aromatic π–π stacking interactions are the only supramolecular interactions seen in all three structures. 相似文献
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4.
Evan R. Moore Andrew E. Bourne Todd J. Hoppe Philip J. Abode Steven R. Boone Gordon H. Purser 《国际化学动力学杂志》2004,36(10):554-564
The mechanism by which an excess of iron(II) ion reacts with aqueous chlorine dioxide to produce iron(III) ion and chloride ion has been determined. The reaction proceeds via the formation of chlorite ion, which in turn reacts with additional iron(II) to produce the observed products. The first step of the process, the reduction of chlorine dioxide to chlorite ion, is fast compared to the subsequent reduction of chlorite by iron(II). The overall stoichiometry is The rate is independent of pH over the range from 3.5 to 7.5, but the reaction is assisted by the presence of acetate ion. Thus the rate law is given by At an ionic strength of 2.0 M and at 25°C, ku = (3.9 ± 0.1) × 103 L mol?1 s?1 and kc = (6 ± 1) × 104 L mol?1 s?1. The formation constant for the acetatoiron(II) complex, Kf, at an ionic strength of 2.0 M and 25°C was found to be (4.8 ± 0.8) × 10?2 L mol?1. The activation parameters for the reaction were determined and compared to those for iron(II) ion reacting directly with chlorite ion. At 0.1 M ionic strength, the activation parameters for the two reactions were found to be identical within experimental error. The values of ΔH? and ΔS? are 64 ± 3 kJ mol?1 and + 40 ± 10 J K?1 mol?1 respectively. © 2004 Wiley Periodicals, Inc. Int J Chem Kinet 36: 554–565, 2004 相似文献
5.
Mohammed I. Jeraal Nicholas Holmes Geoffrey R. Akien Richard A. Bourne 《Tetrahedron》2018,74(25):3158-3164
Reaction optimisation and understanding is fundamental for process development and is achieved using a variety of techniques. This paper explores the use of self-optimisation and experimental design as a tandem approach to reaction optimisation. A Claisen-Schmidt condensation was optimised using a branch and fit minimising algorithm, with the resulting data being used to fit a response surface model. The model was then applied to find new responses for different metrics, highlighting the most important for process development purposes. 相似文献
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7.
A device for aeration and mixing of cell or organelle suspensions in a vertical bore NMR magnet is described. Multiple external sensors (e.g., ion-selective electrodes) may be immersed in the suspension within the bore of the magnet. The sensors are positioned to avoid noise due to contact with gas bubbles and proximity to the probe head. The required sample volume is minimised. The modular design of components permits the use of the device in magnets of various internal dimensions, or with probe heads of different sample tube diameter, by modification of the simpler components of the assembly. 相似文献
8.
Head-to-tail cyclic peptides have been reported to bind to multiple, unrelated classes of receptor with high affinity. They may therefore be considered to be privileged structures. This review outlines the strategies by which both macrocyclic cyclic peptides and cyclic dipeptides or diketopiperazines have been synthesised in combinatorial libraries. It also briefly outlines some of the biological applications of these molecules, thereby justifying their inclusion as privileged structures. 相似文献
9.
Gregory T. Bourne Dr. Daniel J. Kuster Dr. Garland R. Marshall Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(28):8439-8445
Phenylpyridal‐ and phenyldipyridal‐based scaffolds have been designed and synthesized as novel helical peptide mimetics. The synthesis required optimisation and selective alkylation in producing 2,6‐functionalized 3‐hydroxypyridine derivatives for a convergent scheme. The pyridine analogues were coupled by a series of Suzuki/Stille types cross‐coupling reactions. A series of biaryl and ter‐aryl substituted heterocycles were produced. The synthetic approach was concise and high yielding allowing large variability at the wanted side‐chain attachment points. A number of compounds were synthesised to show the versatility of the strategy. 相似文献
10.
Cletus A D'Souza Vikramjit Chopra Richard Varhol Yuan-Yun Xie Slavita Bohacec Yongjun Zhao Lisa LC Lee Mikhail Bilenky Elodie Portales-Casamar An He Wyeth W Wasserman Daniel Goldowitz Marco A Marra Robert A Holt Elizabeth M Simpson Steven JM Jones 《BMC neuroscience》2008,9(1):1-14