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1.
《Journal of Coordination Chemistry》2012,65(18):2884-2895
New macrocyclic complexes were synthesized by template reaction of 1,7-bis(2-formylphenyl)-1,4,7-trioxaheptane, 1,4-bis(2-carboxyaldehydephenoxy)butane or 1,3-bis(2-carboxyaldehydephenoxy)propane with 1,4-bis(2-aminophenoxy)butane, 1,3-bis(2-aminophenoxy)butane, 1,4-bis(4-chloro-2-aminophenoxy)butane or 1,3-bis(4-chloro-2-aminophenoxy)butane and Cu(NO3)2 ·?3H2O or Cu(ClO4)2 ·?6H2O, respectively. The complexes have been characterized by elemental analysis, IR, 1H and 13C NMR, UV–Vis spectra, magnetic susceptibility, conductivity measurements and mass spectra. All complexes are diamagnetic and binuclear. 相似文献
2.
Transition Metal Complexes of 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-Diphosphete 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3aλ5-diphosphete, 1 , reacts with W(CO)6 to yield the isomeric complexes {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)tungsten 4 and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)tungsten 5 . With Cr(CO)6 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)chromium 6 is formed. From the reaction products of Fe3(CO)12 and Fe2(CO)9 with 1 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)iron 7 could be isolated. Properties, nmr, ir and mass spectra of the new compounds are reported. 6 and 7 were characterized by X-ray structure determinations. 相似文献
3.
Synthesis of methylcyclotetra(hexa)siloxanes with different reactive groups at the same silicon atom
N. N. Makarova I. M. Petrova T. V. Vlasova P. V. Petrovskii 《Russian Chemical Bulletin》2006,55(6):968-972
Representatives of methylcyclotetra(hexa)siloxanes with two different reactive groups at the same silicon atom (CH2=CH and Cl, H and Cl, CH2=CH and OH) were synthesized for the first time by condensation of trichlorovinylsilane with dihydroxydimethylsilane, and
by stepwise condensation of trichloro-and trichlorovinylsilane with 1,3-dihydroxy-1,1,3,3-tetramethyldisiloxane in the presence
of amines (aniline, pyridine, and triethylamine). The condensation with 1,3-dihydroxy-1,1,3,3-tetramethyldisiloxane with a
large excess of trichlorosilane, unlike the condensation with trichlorovinylsilane, occured intramolecularly to give monochlorotetramethylcyclotrisiloxane
in a high yield and intermolecularly to give 1,1,7,7-tetrachloro-3,3,5,5-tetramethyl-1,7-dihydrotetrasiloxane. The structures
of the synthesized compounds were confirmed by 1H and 29Si NMR spectroscopy, IR spectroscopy, and mass spectrometry.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 932–936, June, 2006. 相似文献
4.
Augusto Rivera Juan Francisco León Jasmin Rivera Eva Cecilia Parra Jindra Purmova Eleuterio Burgueño-Tapia 《合成通讯》2013,43(11):2029-2040
A one-step synthesis of 2t-substituted-1r,3c-bis(2′-hydroxy-5′- substituted-benzyl)-imidazolidines from 1,3-bis(2′-hydroxy-5′-substituted-benzyl)-imidazolidines and aromatic aldehydes is reported. The relative stereochemistry of the five-membered ring was evident from 1H NMR measurements combined with MMX calculations. 相似文献
5.
Stephanie S. Peterson Tishal Kirby Mariappan Kadarkaraisamy Richard M. Hartshorn Andrew G. Sykes 《Polyhedron》2009,28(14):3031-3035
Reaction of Ag(I) and Cu(I) [M(NCCH3)4]X (X = BF4− and PF6−) salts with 1,8-bis(nicotinyloxy)anthracene-9,10-dione (1), 1,8-bis(isonicotinyloxy)anthracene-9,10-dione (2), and 1,8-bis(pyrimidine-5-carboxyloxy)anthracene-9,10-dione (3), yield new chelating and bridging complexes and two new coordination polymers. The bridging capabilities of ligands 1 and 2 have not been demonstrated before, and ligand 1, by itself, has the flexibility to produce either chelated or bridged structures and an unusual ladder coordination polymer. The tetradentate ligand 3 also produces a one-dimensional coordination polymer in the presence of one equivalent of Ag(I). All complexes have been characterized by X-ray crystallography. 相似文献
6.
Z. Asfari S. Wenger J. Vicens 《Journal of inclusion phenomena and macrocyclic chemistry》1994,19(1-4):137-148
The synthesis of 1,2- and 1,3-calix[4]-bis-crowns, double calix[4]arenes and double calixcrowns have been shown to depend on the reaction conditions (nature of the base, structure of the ditosylates, and the stoichiometry of the reactants). The 1,3-alternate conformation of the 1,3-calix[4]-bis-crowns was shown to be favourable to the selective complexation of cesium cation. The observed Na+/Cs+ selectivity was exploited in separation processes using them as carriers in transport through supported liquid membranes (SLMs). The best Na+/Cs+ selectivity (1/45 000) was observed for the naphthyl derivative 7. Calix(aza) crowns and 1,3-calix[4]-bis-(aza)-crowns were also produced through the preliminary formation of the Schiff base-calixarenes, which were further hydrogenated. The syntheses consisted of the 1,3-selective alkylation of calixarenes followed by cyclization into a 1,3-bridged calixarene or by the direct 1,3-capping of the calixarene with appropriate ditosylates. Soft metal complexation by these ligands is also presented.This paper is dedicated to the commemorative issue on the 50th anniversary of calixarenes. 相似文献
7.
L. V. Klyba E. R. Sanzheeva L. G. Shagun L. V. Zhilitskaya 《Russian Journal of Organic Chemistry》2017,53(8):1233-1238
By the method of nanostructure-assisted laser desorption/ionization (NALDI) analysis was performed of solid and liquid fractions of reaction products formed from 2-methylimidazole and 1,3-bis- (iodomethyl)-1,1,3,3-tetramethyldisiloxane. Basing on the data post-source decay of iodides major and minor products of reaction were identified that were registered as ions [M–I]+ and [M–I3]+. 相似文献
8.
Heike Hund Gerd-Volker Röschenthaler 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):71-74
Abstract In an oxidative addition reaction O,O′-bis(trimethylsilyl)diacetyldioxime 2 and triethylphosphite give 1,3,2-Δ5[sgrave]5-diazaphospholene 3a which hydrolyzes to form (Z)-2,3-bis(hydroxylamino)-2-butene 4. Benzaldehyde and 4 condensate to furnish 1,3-dihydroxy-4,5-dimethyl-2-dimethyl-4-imidazoline 5. Tris(trimethylsilyl)phosphite and 2 react to give the first tris(trimethylsiloxy)phosphorane 3b. 相似文献
9.
《Journal of Coordination Chemistry》2012,65(23):2509-2517
13,14-bis(Hydroxyimino)-4,7-bis(ferrocenylmethyl)-2,3,4,5,6,7,8,9-octahydrobenzo[k]-4, 7-diaza-1,10-dithiacyclododecine[13,14-g]-quinoxaline (H2L) has been prepared from (E,E)-dichloroglyoxime and 12,13-diamino-4,7-bis(ferrocenylmethyl)-2,3,4,5,6,7,8,9-octahydrobenzo[k]-4,7-diaza-1,10-dithiacyclododecine which was synthesized from 12,13-dinitro-4,7-bis(ferrocenylmethyl)-2,3,4,5,6,7,8,9-octahydrobenzo[k]4,7-diaza-1,10-dithia cyclododecine. Mononuclear nickel(II) and copper(II) complexes of H2L have a metal-ligand ratio of 1?:?2 and the ligand coordinates through two nitrogen atoms, as do most (E,E)-dioximes. The homotrinuclear [Cu(L)2Cu2(dipy)2](NO3)2 compound coordinates to the other two copper(II) ions through deprotonated oximate oxygens and two 2,2′-dipyridyl as an end-cap ligand to yield the trinuclear structure. The ligand and its complexes have been characterized on the basis of 1H, 13C NMR, IR and MS spectroscopy and elemental analyses. 相似文献
10.
Yvonne Zimmermann Mohamed El-Sayed Silvio Prause Stefan Spange 《Monatshefte für Chemie / Chemical Monthly》2001,10(3):1347-1361
Kamlet-Taft’s α (hydrogen bond donor acidity) and π* (dipolarity/polarizability) values of various silica batches measured in various solvents are presented. The α and π* parameters for the various solid acids are analyzed by means of Fe(phen)2(CN)2 (cis-dicyano-bis-(1,10)-phenanthroline-iron(II), 1), Michler’s ketone (4,4′-bis-(dimethylamino)-benzophenone, 2), and two hydrophilic derivatives of 2, (4-(dimethylamino)-4′-(di-2-hydroxyethyl)-amino-benzophenone (3a) and 4,4′-bis-(di-(2-hydroxyethyl)-amino)-benzophenone (3b) as well as coumarin 153 (4) as solvatochromic surface polarity indicators. Apparent β (hydrogen bond acceptor basicity) parameters for bare silica have been evaluated by means of an aminobenzodifuranone dye (5) as solvatochromic probe. The chemical interpretation of the α and π* parameters and the nature of the solvent/surface interaction which they reflect are discussed. It can be shown that an increase of the HBA (hydrogen bond accepting) capacity of the solvent significantly decreases the HBD (hydrogen bond donating) capacity of the surface environment, whereas the dipolarity/polarizability value of the silica/solvent interface is a composite of many effects. The classification of the polarity of silica particles in organic solvents compared to pure liquids is outlined. 相似文献
11.
Zekeriya Bıyıklıoğlu Beytullah Ertem Selami Karslıoğlu Yaşar Gök 《Transition Metal Chemistry》2007,32(5):591-596
The novel (E,E)-dioxime,7,8-bis(hydroxyimino)-1,14-bis(monoaza[8]crown-6)-benzo[f]-4,11-dioxa-1,14-diazadecane[7,8-g]quinoxaline (H2L), has been synthesized by the reaction of 6,7-diamino-1,12-bis(monoaza[18]crown-6)benzo[f]-4,9-dioxa-1,12-diazadecane (4) which has been prepared by the reduction of 6,7-dinitro-1,12-bis(mono-aza[18]crown-6)benzo[f]-4,9-dioxa-1,12-diazdecane (3) and cyanogendi-N-oxide. Mononuclear NiII and CuII complexes of H2L have a metal:ligand ratio of 1:2 and the ligand coordinates through two hydroxyimino nitrogen atoms, as do most of the (E,E)-dioximes. The hydrogen-bridged NiII complex was converted into its BF
2
+
capped anologue by the reaction with BF3 · Et2O. The reaction of the CuII complex with 2,2′-dipyridyl as an end-cap ligand gave the homotrinuclear complex. Structures for the ligand and its complexes
are proposed in accordance with elemental analysis, magnetic susceptibility measurements, 1H, 13C-n.m.r, IR and MS spectral data. 相似文献
12.
Chikkanti Jaganmohan Vinay Kumar K. P. Sandeep Reddy G. Sandeep Mohanty Jaydeep Kumar Venkateswara Rao B. 《合成通讯》2018,48(2):168-174
A new versatile and efficient strategy for the synthesis of 2,2-bis(dimethylamino)-3-alkyl or benzyl 2,3-dihydroquinazoline-4(1H)-one compounds has been developed by one-pot multicomponent reaction with isatoic anhydride, amines followed by in situ-generated Vilsmeier reagent. The reaction has also been studied with different amines and solvents. 相似文献
13.
A (Phosphonioalkinyl)- and an Acetyl(tetracarbonyl)iron From the reaction of 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1 , and Fe(CO)5 {[bis(dimethylamino)phosphoryl-methyl]-bis(dimethylamino)phosphonioethinyl}(tetracarbonyl)iron, 4 , and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro- 1λ5,3λ5-[1,3]diphosphetium-2-carbonyl}(tetracarbonyl)-iron, 5 , can be isolated as crystalline products. The nmr, mass and ir spectra of the two compounds as well crystal and molecular structures of 4 are reported. The bonding situation in compounds 4 and 5 are discussed in detail. 相似文献
14.
László Jánosi László Kollár Piero Macchi Angelo Sironi 《Transition Metal Chemistry》2007,32(6):746-752
Pt(diphosphine)X(aryl) complexes [diphosphine = 1,3-bis(diphenylphosphino)propane (dppp), 2,4-bis(diphenylphos phino)pentane (bdpp); aryl = phenyl, 2-thiophenyl; X = Cl, I] have been reacted with ethyl diazoacetate in chloroform.
It has been revealed by in␣situ n.m.r. studies that the starting compounds insert the carbene, formed from ethyl diazoacetate, into the Pt–aryl group resulting
in Pt(diphosphine)X{CH(aryl)COOC2H5}. Depending on the reaction conditions (reaction time, ratio of the reactants) and the ligands various side-reactions have
been observed: (i) the formation of Pt(diphosphine)X2 in chloroform, (ii) the insertion of the :CHCOOC2H5 fragment into the Pt–halide bond of the dihalogeno complexes Pt(diphosphine)X2 resulting in the exclusive formation of Pt(diphosphine)X(CHXCOOC2H5). Diastereoselective insertion reactions have been observed in the presence of (S,S)-bdpp as diphosphine. The Pt{(S,S)-bdpp)}I(Ph) complex has been characterized by X-ray crystallography. 相似文献
15.
Yvonne Zimmermann Mohamed El-Sayed Silvio Prause Stefan Spange 《Monatshefte für Chemie / Chemical Monthly》2001,132(11):1347-1361
Summary. Kamlet-Taft’s α (hydrogen bond donor acidity) and π* (dipolarity/polarizability) values of various silica batches measured in various solvents are presented. The α and π* parameters for the various solid acids are analyzed by means of Fe(phen)2(CN)2 (cis-dicyano-bis-(1,10)-phenanthroline-iron(II), 1), Michler’s ketone (4,4′-bis-(dimethylamino)-benzophenone, 2), and two hydrophilic derivatives of 2, (4-(dimethylamino)-4′-(di-2-hydroxyethyl)-amino-benzophenone (3a) and 4,4′-bis-(di-(2-hydroxyethyl)-amino)-benzophenone (3b) as well as coumarin 153 (4) as solvatochromic surface polarity indicators. Apparent β (hydrogen bond acceptor basicity) parameters for bare silica have
been evaluated by means of an aminobenzodifuranone dye (5) as solvatochromic probe.
The chemical interpretation of the α and π* parameters and the nature of the solvent/surface interaction which they reflect are discussed. It can be shown that an increase
of the HBA (hydrogen bond accepting) capacity of the solvent significantly decreases the HBD (hydrogen bond donating) capacity
of the surface environment, whereas the dipolarity/polarizability value of the silica/solvent interface is a composite of
many effects. The classification of the polarity of silica particles in organic solvents compared to pure liquids is outlined.
Theoretical E
T(30) values of the solid/solvent interfaces are calculated by applying linear solvation energy (LSE) relationships using the
independently measured α and π* values of the solid acids according to
Received February 2, 2001. Accepted (revised) March 3, 2001 相似文献
16.
17.
J. A. Moore T. D. Mitchell 《Journal of polymer science. Part A, Polymer chemistry》1983,21(5):1305-1314
Polyenaminoesters were prepared by condensation of succinyl succinic ester (SSE) and p-bis-carbomethoxy diacetyl benzene (CDB) with 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane. Conditions of solvent and temperature were discovered which yielded soluble polymer from SSE after heat treatment. CDB yields only tough, rubbery, insoluble products. 相似文献
18.
Fred Rosche Gernot Heckmann Ekkehard Fluck Bernhard Neumüller 《Heteroatom Chemistry》1996,7(5):341-347
1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, reacts with diphenylchlorophosphane to yield 1,1,3,3-tetrakis(dimethylamino)-4-diphenylphosphanyl-1,2-dihydro-3λ5-[1,3]diphosphetium chloride, 2, or, depending on the reaction conditions, the isomer compound 3. The cation of 2 is deprotonated by LiN[Si(CH3)3]2 to give the diphenylphosphanyl-substituted derivative of 1, i.e., compound 4. Methyl iodide adds to 1 to form 1,1,3,3-tetrakis(dimethylamino)-4-methyl-1,2-dihydro-3λ5-[1,3]diphosphetium iodide, 6. Deprotonation of 6 with n-butyllithium leads to the monomethyl derivative of 1, i.e., compound 7. Physical properties, NMR spectra, and mass spectra of compounds 2–4, 6, and 7 are described. The results of the X-ray structural analysis of 6 are reported and discussed. © 1996 John Wiley & Sons, Inc. 相似文献
19.
P. Thuéry M. Nierlich C. Bressot V. Lamare J. F. Dozol Z. Asfari J. Vicens 《Journal of inclusion phenomena and macrocyclic chemistry》1995,23(4):305-312
The crystal structures of two binuclear complexes between caesium and 1,3-calix[4]-bis-crowns have been determined. Cs2
Bis-benzoC6(NO3)2. 3CHCl3 (1) in whichBis-benzoC6 is 1,3-calix[4]-bis-benzo-crown-6, crystallizes in the orthorhombic system: space groupPca2
1 a=19.513(10),b=15.382(5),c=23.708(9) Å,V=7116(5) Å3,Z=4. Refinement led to a final conventionalR value of 0.065 for 2321 reflections. The structure of (1) is analogous to those already reported withBis-C6, (in whichBis-C6 is, 1,3-calix[4]-bis-crown-6) and NO
3
–
as a counter-ion. Cs2
Bis-C6(NCS)2 (2) crystallizes in the monoclinic system: space, groupC2 a=36.57(2),b=11.47(1),c=13.65(1) Å, =109.03(5)°.,V=5415(6) Å3,Z=4. Refinement led to a final conventionalR value of 0.063 for 2227 reflections. Compound (2) is made of dimers bridged by a disordered NCS– ion. The crown ether chain conformations are discussed.
Supplementary data relating to this article (atomic coordinates, anisotropic displacement parameters, bond distances and angles and observed and calculated structure factors) are deposited with the British Library as Supplementary Publication No. SUP 82199 (52 pages). 相似文献
20.
《Journal of Coordination Chemistry》2012,65(3-4):335-342
Abstract On reacting 1,2-bis(diphenylphosphino)ethanedichloropalladium(II) with equimolar amount of silver perchlorate, a binuclear complex, di-μ-chloro-bis[1,2-bis(diphenylphosphino)ethane-palladium(II)] (1) is formed. The crystal structure of 1 has been solved. It crystallizes with two chloroform molecules. Chloro bridges are symmetrical and normal (Pd-Cl~2.414(3) Å). The immediate environment around palladium is slightly distorted square planar and the P-Pd-P angle is ~85°. IR bands at 290 and 270cm?1 are observed for the chloro-bridged core of the complex. 相似文献