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1.
Minoo Dabiri Peyman Salehi Mostafa Baghbanzadeh 《Monatshefte für Chemie / Chemical Monthly》2007,43(7):1191-1194
2,3-Dihydroquinazolin-4(1H)-ones were efficiently synthesised by the reaction of isatoic anhydride, a primary amine or ammonium acetate, and different
aromatic aldehydes in 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim]BF4) without using any acidic catalyst. Also a bis-derivative of the title compound as a polyheterocyclic system was synthesised
successfully in high yield. 相似文献
2.
Aurkie Ray Sambuddha Banerjee Georgina M. Rosair Volker Gramlich Samiran Mitra 《Structural chemistry》2008,19(3):459-465
A nickel(II) and a cobalt(III) complex of two different potentially tetradentate Schiff bases with different binding modes
have been synthesised. The nickel(II) complex [NiL1] · CH3OH (1) was formed, on reacting the metal salt with a perfectly symmetrical N2O2 tetradentate Schiff base ligand H
2
L
1
, which is the 1:2 condensation product of 1,3-diamino propane and 2-hydroxyacetophenone. The cobalt(III) complex [Co(HL2)3] · (ClO4)3 · H2O (2) was synthesised using an asymmetric N2O2 tetradentate Schiff base ligand HL
2
on condensing N,N-dimethyl-1,3-diamino propane with o-vanillin in 1:1 mmol ratio. Although both Schiff bases are N2O2 functionalised, they showed variation in their coordinative property with nickel(II) and cobalt(III) ions. Both the complexes
were characterised by IR spectroscopy and cyclic voltammetry and their single crystal structures clearly indicate that 1 is a mononuclear species whereas 2 is a hydrogen-bonded dimer. 相似文献
3.
Summary. The two new compounds Mn(dien)2[MoS4] (1) and Mn(dien)2[Mo2O2S6] (2) (dien = diethylenetriamine) were prepared under solvothermal conditions. Both compounds were obtained as phase-pure products. The
structures consist of new [Mn(dien)2]2+ cations and isolated tetrahedral [MoS4]2− (1) or [Mo2O2S6]2− (2) anions. Between the anions and the cations, hydrogen bonding is observed. Compound 1 crystallizes in the tetragonal space group I (a = 10.219(2), c = 9.259(2) ?, Z = 2), whereas 2 crystallizes in the monoclinic space group P21/c (a = 8.703(2), b = 18.390(4), c = 14.603(3) ?, β = 103.18(3)°, Z = 4). The thermal behaviour of the thiomolybdates was investigated using difference thermoanalysis (DTA) and thermogravimetry
(TG). Both compounds decompose under argon with a single endothermic signal in the DTA curve (peak maximum: 252 (1) and 242°C (2)).
Received November 5, 2001. Accepted December 27, 2001 相似文献
4.
Kinetico‐Mechanistic Insights on the Assembling Dynamics of Allyl‐Cornered Metallacycles: The PtNpy Bond is the Keystone
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Dr. Inmaculada Angurell Dr. Montserrat Ferrer Dr. Albert Gutiérrez Prof. Manuel Martínez Dr. Mercè Rocamora Dr. Laura Rodríguez Prof. Oriol Rossell Dipl.‐Chem. Yvonne Lorenz Dr. Marianne Engeser 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(44):14473-14487
The square‐like homo‐ and heterometallamacrocycles [{Pd(η3‐2‐Me‐C3H4)( L n )2}2{M(dppp)}2](CF3SO3)6 (dppp=1,3‐bis(diphenylphosphino)propane) and [{Pd(η3‐2‐Me‐C3H4)( L1 )2}2{M(PPh3)2}2](CF3SO3)6 [py=pyridine, M=Pd, Pt, L n =4‐PPh2py ( L1 ), 4‐C6F4PPh2py ( L2 )] containing allyl corners were synthesised by antisymbiotic self‐assembly of the different palladium and platinum metallic corners and the ambidentate N,P ligands. All the synthesised assemblies displayed a complex dynamic behaviour in solution, the rate of which is found to be dependent on the electronic and/or steric nature of the different building blocks. A kinetico‐mechanistic study by NMR line shape analysis of the dynamics of some of these assemblies was undertaken in order to determine the corresponding thermal activation parameters. Both an enhanced thermodynamic stability and slower dynamics were observed for platinum‐pyridine‐containing species when compared with their palladium analogues. Time‐dependent NMR spectroscopy in combination with ESI mass spectrometry was used to study the exchange between the assemblies and their building blocks, as well as that occurring between different metallamacrocycles. Preliminary studies were carried out on the activity of some of the metallamacrocyclic compounds as catalytic precursors in the allylic substitution reaction, and the results compared with that of the monometallic allylic corner [Pd(η3‐2‐Me‐C3H4)( L1 )2]+. 相似文献
5.
Summary. A series of ureidopropenenitriles were synthesised by Knoevenagel condensation of ArCOCH2CN and HC(OEt)3 in presence of ureas in a one pot reaction. These ureidopropenenitriles were cyclised to 4-aryl-5-cyano-3-substituted pyrimidines (in acid) or to 4-amino-5-benzoylpyrimidines (in base) in 60–70% yields. The amine pyrimidine derivatives were further converted to substituted uracils by hydrolysis with isopentyl nitrite in DMF. Alkylation of uracils furnished 1,3-dimethyluracil derivatives with DMS in alkali. All new compounds were characterised by spectral and analytical methods. 相似文献
6.
Reinout Meijboom Marco Haumann Andreas Roodt Llewellyn Damoense 《Helvetica chimica acta》2005,88(3):676-693
The dinuclear complex [Co2(CO)6{P(O‐2,4‐t‐Bu2C6H3)3}2] ( 6 ) has been synthesised and fully characterised. X‐Ray crystal‐structure analysis revealed a trans‐diaxial geometry, no bridging carbonyls, and Co? Co and Co? P bond lengths of 2.706(5) and 2.134(4) Å, respectively. The hydroformylation of pent‐1‐ene in the presence of 6 was studied at 120–180° at pressures between 20 and 80 bar Syngas. High‐pressure (HP) spectroscopy (IR, NMR) was used to detect potential hydride intermediates. HP‐IR Studies revealed the formation of [CoH(CO)3{P(O‐2,4‐t‐Bu2C6H3)3}] ( 2 ) at ca. 105°, with no significant amount of [CoH(CO)4] detectable. The intermediate 2 was synthesised and characterised. The formation of the undesired complex [CoH(CO)2{P(O‐2,4‐t‐Bu2C6H3)3}2] was completely suppressed due to the large cone angle of the sterically demanding phosphite. 相似文献
7.
Lewis C. Wilkins Dr. James R. Lawson Philipp Wieneke Frank Rominger Prof. Dr. A. Stephen K. Hashmi Dr. Max M. Hansmann Dr. Rebecca L. Melen 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(41):14618-14624
A diverse range of Lewis acidic alkyl, vinyl and aryl boranes and borenium compounds that are capable of new carbon–carbon bond formation through selective migratory group transfer have been synthesised. Utilising a series of heteroleptic boranes [PhB(C6F5)2 ( 1 ), PhCH2CH2B(C6F5)2 ( 2 ), and E‐B(C6F5)2(C6F5)C=C(I)R (R=Ph 3 a , nBu 3 b )] and borenium cations [phenylquinolatoborenium cation ([QOBPh][AlCl4], 4 )], it has been shown that these boron‐based compounds are capable of producing novel allyl‐ boron and boronium compounds through complex rearrangement reactions with various propargyl esters and carbamates. These reactions yield highly functionalised, synthetically useful boron substituted organic compounds with substantial molecular complexity in a one‐pot reaction. 相似文献
8.
Almut Haberer Reinhard Kaindl Jürgen Konzett Robert Glaum Hubert Huppertz Prof. Dr. 《无机化学与普通化学杂志》2010,636(7):1326-1332
Er5(BO3)2F9 was synthesised under conditions of 3 GPa and 800 °C in a Walker‐type multianvil apparatus. The crystal structure was determined on the basis of single‐crystal X‐ray diffraction data, collected at room temperature. Er5(BO3)2F9 is isotypic to the recently synthesised Yb5(BO3)2F9 and crystallises in C2/c with the lattice parameters a = 2031.2(4) pm, b = 609.5(2) pm, c = 824.6(2) pm, and β = 100.29(3)°. The physical properties of RE5(BO3)2F9 (RE = Er, Yb) including high temperature behaviour and single crystal IR‐ / Raman spectroscopy were investigated. 相似文献
9.
Helge Klare Sebastian Hanft Dr. Jörg M. Neudörfl Dr. Nils E. Schlörer Prof. Dr. Axel Griesbeck Prof. Dr. Bernd Goldfuss 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(37):11847-11855
Modular cyclodiphosph(V)azanes are synthesised and their affinity for chloride and actetate anions were compared to those of a bisaryl urea derivative ( 1 ). The diamidocyclodiphosph(V)azanes cis‐[{ArNHP(O)(μ‐tBu)}2] [Ar=Ph ( 2 ) and Ar=m‐(CF3)2Ph ( 3 )] were synthesised by reaction of [{ClP(μ‐NtBu)}2] ( 4 ) with the respective anilines and subsequent oxidation with H2O2. Phosphazanes 2 and 3 were obtained as the cis isomers and were characterised by multinuclear NMR spectroscopy, FTIR spectroscopy, HRMS and single‐crystal X‐ray diffraction. The cyclodiphosphazanes 2 and 3 readily co‐crystallise with donor solvents such as MeOH, EtOH and DMSO through bidentate hydrogen bonding, as shown in the X‐ray analyses. Cyclodiphosphazane 3 showed a remarkably high affinity (log[K]=5.42) for chloride compared with the bisaryl urea derivative 1 (log[K]=4.25). The affinities for acetate (AcO?) are in the same range ( 3 : log[K]=6.72, 1 : log[K]=6.91). Cyclodiphosphazane 2 , which does not contain CF3 groups, exhibits weaker binding to chloride (log[K]=3.95) and acetate (log[K]=4.49). DFT computations and X‐ray analyses indicate that a squaramide‐like hydrogen‐bond directionality and Cα?H interactions account for the efficiency of 3 as an anion receptor. The Cα?H groups stabilise the Z,Z‐ 3 conformation, which is necessary for bidentate hydrogen bonding, as well as coordinating with the anion. 相似文献
10.
Tatyana Saplinova Vadym Bakumov Tobias Gmeiner Jörg Wagler Marcus Schwarz Edwin Kroke Prof. Dr. 《无机化学与普通化学杂志》2009,635(15):2480-2487
The title compound C6N7(NHNH2)3 ( 1 ) was obtained from melem C6N7(NH2)3 or melon [C6N7(NH2)NH]n and hydrazine by an autoclave synthesis. Upon treatment with a 10 % HCl solution it is transformed into the trihydrochloride [C6N7(NHNH3)3]Cl3 ( 2 ). Compounds 1 and 2 were analysed with 13C NMR, 15N NMR, FTIR and Raman spectroscopy. Furthermore, the single‐crystal X‐ray structure of the pentahydrate of 2 is reported (P\bar{1} , a = 674.96(3), b = 1214.17(6), c = 1272.15(6) pm, α = 66.288(2)°, β = 75.153(2)°, γ = 80.420(2)°, V = 920.30(8)·106 pm3, Z = 2, T = 90(2) K). The thermal decomposition of 1 and 2 was investigated with TG/DTA. Reaction of 1 with NaNO2/HCl yields triazido‐s‐heptazine, C6N7(N3)3 ( 3 ). Tris(tri‐n‐butylphosphinimino)‐s‐heptazine ( 4 ) was synthesised from 3 and characterised by means of 13C, 31P, 1H NMR, FTIR and MALDI‐TOF spectroscopy. Similar to s‐heptazine derivative 3 , compounds 1 and 4 are precursors for graphitic carbon nitrides, which have attracted considerable attention recently, and to various potential applications, such as flame retardants and (photo) catalysis. 相似文献
11.
Dirk Steinborn Tobias Hoffmann Michael Gerisch Clemens Bruhn Harry Schmidt Karsten Nordhoff Julian A. Davies Kristin Kirschbaum Ingo Jolk 《无机化学与普通化学杂志》2000,626(3):661-666
The platina‐β‐diketones [Pt2{(COR)2H}2(μ‐Cl)2] ( 1 , R = Me a , Et b ) react with phosphines L in a molar ratio of 1 : 4 through cleavage of acetaldehyde to give acylplatinum(II) complexes trans‐[Pt(COR)Cl(L)2] ( 2 ) (R/L = Me/P(p‐FC6H4)3 a , Me/P(p‐CH2=CHC6H4)Ph2 b , Me/P(n‐Bu)3 c , Et/P(p‐MeOC6H4)3 d ). 1 a reacts with Ph2As(CH2)2PPh2 (dadpe) in a molar ratio of 1 : 2 through cleavage of acetaldehyde yielding [Pt(COMe)Cl(dadpe)] ( 3 a ) (configuration index: SP‐4‐4) and [Pt(COMe)Cl(dadpe)] (configuration index: SP‐4‐2) ( 3 b ) in a ratio of about 9 : 1. All acyl complexes were characterized by 1H, 13C and 31P NMR spectroscopy. The molecular structures of 2 a and 3 a were determined by single‐crystal X‐ray diffraction. The geometries at the platinum centers are close to square planar. In both complexes the plane of the acyl ligand is nearly perpendicular to the plane of the complex (88(2)° 2 a , 81.2(5)° 3 a ). 相似文献
12.
Dayse N. Moreira Clarissa P. Frizzo Kelvis Longhi Nilo Zanatta Helio G. Bonacorso Marcos A. P. Martins 《Monatshefte für Chemie / Chemical Monthly》2008,139(9):1049-1054
The synthesis of eleven 1-cyanoacetyl-5-hydroxy-5-halomethyl-4,5-dihydro-1H-pyrazoles from the reaction of 4-alkoxy-3-alken-2-ones f(R
3C(O)C(R
2) = C(R
1)OR, where R
3 = CF3, CCl3, CHCl2, CO2
Et; R
2/R
1 = H/H, H/Me, H/Et, -(CH2)4-, Me/H, H/Pr, and R = Me, Et) with cyanoacetohydrazide is reported. The reaction was carried out in the ionic liquid ([bmim][BF4]) and molecular solvents. The results showed that when the ionic liquid was used as reaction medium, the reaction time was
drastically decreased and the yield was improved.
Correspondence: Marcos A. P. Martins, Núcleo de Química de Heterociclos – NUQUIMHE, Universidade Federal de Santa Maria, Santa
Maria, RS, Brazil. 相似文献
13.
4‐Fluorinated levoglucosans were synthesised to test if OH???F H‐bonds are feasible even when the O???F distance is increased. The fluorinated 1,6‐anhydro‐β‐D ‐glucopyranoses were synthesised from 1,6 : 3,4‐dianhydro‐β‐D ‐galactopyranose ( 8 ). Treatment of 8 with KHF2 and KF gave 43% of 4‐deoxy‐4‐fluorolevoglucosan ( 9 ), which was transformed into the 3‐O‐protected derivatives 13 by silylation and 15 by silylation, acetylation, and desilylation. 4‐Deoxy‐4‐methyllevoglucosan ( 19 ) and 4‐deoxylevoglucosan ( 21 ) were prepared as reference compounds that can only form a bivalent H‐bond from HO? C(2) to O? C(5). They were synthesised from the iPr3Si‐protected derivative of 8 . Intramolecular bifurcated H‐bonds from HO? C(2) to F? C(4) and O? C(5) of the 4‐fluorinated levoglucosans in CDCl3 solution are evidenced by the 1H‐NMR scalar couplings h1J(F,OH) and 3J(H,OH). The OH???F H‐bond over an O???F distance of ca. 3.0 Å is thus formed in apolar solvents, at least when favoured by the simultaneous formation of an OH???O H‐bond. 相似文献
14.
The four isomeric 3-dimethylamino-trans-2-decalols-1,1,4,4-d4 have been synthesised. Examination of PMR spectra of these compounds allows us to confirm the ‘flattened-chair’ conformation for the cis N(CH3)2a OHe isomer, whereas the remaining three conserve the double chair conformation. The same type of flattening is also observed in the case of the diaxial quaternary ammonium salt and is even more marked in the cis N(CH3)3a OHe isomer resulting in a ‘twist-chair’ conformation. 相似文献
15.
Ahmed Jasim M. Al-Karawi 《Liquid crystals》2017,44(14-15):2285-2300
Continuation with our previous investigation which refers to the synthesis of a series of hydrophobic symmetrical azine compounds: 1,2-bis[4-(n-alkoxy)benzylidene]hydrazine (where, n-alkoxy: O(CH2)nH, n = 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12, 16 or 18), a series of hydrophobic asymmetrical azine compounds: [1-(4-propyloxy)-2-(4?-(n-alkoxy))benzylidene]hydrazine (where, n-alkoxy: O(CH2)nH, n = 1, 2, 4, 5, 6, 7, 8, 9, 10, 12, 16 or 18) was synthesised following an efficient and practical method. These compounds were synthesised by the condensation reaction of hydrazine hydrate with 4-propyloxybenzaldehyde and appropriately 4-(n-alkoxy)benzaldehydes in acidic medium and ambient conditions (very simple way with no need of any sophisticated techniques). Moreover, two new series of silver(I) complexes based on symmetrical or asymmetrical azines have been synthesised (linear-binuclear type complexes with the general formula [Ag2(L)(NO3)2] were obtained). The organic compounds and their silver(I) complexes were characterised using different techniques: microelemental analysis and spectral data (FTIR, UV–Vis, 1HNMR, 13C{1H}NMR, 2D 1H-1H-COSY, 2D 1H-13C-HSQC and mass spectra) as well as molar conductivity measurements for silver(I) complexes. Liquid crystal behaviour of the prepared compounds were studied using polarised light optical microscopy and confirmed with differential scanning calorimetry and X-ray powder diffraction techniques. The studies revealed that all azine compounds and some of silver(I) complexes are liquid crystal materials. The luminescent properties of all the prepared compounds were also investigated which confirmed that all of these compounds are photo-luminescent in the crystalline solid state and in the mesophase. 相似文献
16.
Cs[Na(NH3)6][B10H10]·NH3 was synthesised from cesium and disodium‐decahydro‐closo‐decaborate Na2B10H10 in liquid ammonia, from which it crystallized in form of temperature sensitive colorless plates (triclinic, P1¯, a = 8.4787(7) Å, b = 13.272(1) Å, c = 17.139(2) Å, α = 88.564(1)°, β = 89.773(1)°, γ = 81.630(1)°, V = 1907.5(3) Å3, Z = 4). The compound is the first example of an alkali metal boranate with two different types of cations. The decahydro‐closo‐decaborate dianions [B10H10]2— and the cesium cations form a equation/tex2gif-stack-1.gif[Cs2(B10H10)2]2— layer parallel to the ac plane. These layers are separated by N—H···N‐hydrogen bonded hexamminesodium cations. 相似文献
17.
Botjan Japelj Simon Re
nik Petra ebaek Branko Stanovnik Jurij Svete 《Journal of heterocyclic chemistry》2005,42(6):1167-1173
A series of alkyl l‐heteroaryl‐1H‐1,2,3‐triazole‐4‐carboxylates 6a‐u were synthesised in four steps from methyl (Z)‐2‐benzyloxycarbonylarmino‐3‐(dimethylamino)prop‐2‐enoate ( 1 ) and heterocyclic amines 2a‐s. Triazoles 6a‐o were tested against antimycobacterial activity. For the most active compound, n‐pentyl 1‐(6‐phenylpyridazin‐3‐yl)‐1H‐1,2,3‐triazole‐4‐carboxylate ( 6n ), minimum inhibitory concentration 3.13 μg/ml was determined. 相似文献
18.
T. G. Drushlyak L. A. Kutulya N. S. Pivnenko V. V. Vashchenko 《Russian Journal of General Chemistry》2005,75(4):622-627
Carbonylation of (E)-2-(4-halobenzylidene)-p-menthan-3-ones, catalyzed by PdCl2(PPh3)2, gave a distereometric mixure of 4-[(1R,4R)- and (1R,4S)-3-oxo-p-menthan-2-ylidenemethyl]benzoic acids, whose reaction with phenols gave 1R,4R diastereomers of the corresponding esters.__________Translated from Zhurnal Obshchei Khimii, Vol. 75, No. 4, 2005, pp. 659–664.Original Russian Text Copyright © 2005 by Drushlyak, Kutulya, Pivnenko, Vashchenko. 相似文献
19.
Daiji Ogata Junpei Yuasa 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(51):18595-18599
This work demonstrates a new nonconventional ligand design, imidazole/pyridine‐based nonsymmetrical ditopic ligands ( 1 and 1 S ), to construct a dynamic open coordination cage from nonsymmetrical building blocks. Upon complex formation with Pd2+ at a 1:4 molar ratio, 1 and 1 S initially form mononuclear PdL4 complexes (Pd2+( 1 )4 and Pd2+( 1 S )4) without formation of a cage. The PdL4 complexes undergo a stoichiometrically controlled structural transition to Pd2L4 open cages ((Pd2+)2( 1 )4 and (Pd2+)2( 1 S )4) capable of anion binding, leading to turn‐on anion binding. The structural transitions between the Pd2L4 open cage and the PdL4 complex are reversible. Thus, stoichiometric addition (2 equiv) of free 1 S to the (Pd2+)2( 1 S )4 open cage holding a guest anion ((Pd2+)2( 1 S )4?G?) enables the structural transition to the Pd2+( 1 S )4 complex, which does not have a cage and thus causes the release of the guest anion (Pd2+( 1 S )4+G?). 相似文献
20.
Johannes Krebs Martin Haehnel Dr. Ivo Krummenacher Dr. Alexandra Friedrich Prof. Dr. Holger Braunschweig Prof. Dr. Maik Finze Prof. Dr. Lei Ji Prof. Dr. Todd B. Marder 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(31):8159-8167
Bis(1-(4-tolyl)-carboran-2-yl)-(4-tolyl)-borane [(1-(4-MeC6H4)-closo-1,2-C2B10H10-2-)2(4-MeC6H4)B] ( 1 ), a new bis(o-carboranyl)-(R)-borane was synthesised by lithiation of the o-carboranyl precursor and subsequent salt metathesis reaction with (4-tolyl)BBr2. Cyclic voltammetry experiments on 1 show multiple distinct reduction events with a one-electron first reduction. In a selective reduction experiment the corresponding paramagnetic radical anion 1.− was isolated and characterized. Single-crystal structure analyses allow an in-depth comparison of 1 , 1.− , their calculated geometries, and the S1 excited state of 1 . Photophysical studies of 1 show a charge transfer (CT) emission with low quantum yield in solution but a strong increase in the solid state. TD-DFT calculations were used to identify transition-relevant orbitals. 相似文献