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1.
Janaína Marques Rodrigues Carlos Mauricio R. Sant’Anna Victor Marcos Rumjanek João Batista Neves DaCosta 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):40-56
A series of 22 dialkylphosphorylydrazones (dialkyl ester, N′-[(1E)-(R1 phenyl)methylene]-phosphorohydrazidic acid), 20 of them new, along with three new N,N′-bis (diisobutylphosphorylthioamide)diamines (bis-[diisobutyl ester), N-thioxomethylene]-, diamine)phosphora-midic acid, were prepared and characterized by IR, 1H NMR, 13C NMR, 31P NMR, and mass spectrometry. The analysis of 1H NMR, 13C NMR, 31P NMR, and NOE spectra confirmed the observation of the single diastereoisomer E in the synthesis of dialkylphosphorylydrazones. The results of a molecular modeling study performed in order to investigate the mechanism of the synthesis of dialkylphosphorylydrazones are in agreement with the experimental results, i.e., the favored formation of diastereoisomer E over Z. 相似文献
2.
Poly(alkylene phosphate)s bearing regularly distributed uracil moiety in the main chain have been obtained. The synthetic procedure consists of condensation of bis(diethylamino)-methoxyphosphine with N1,N3-bis(2′-hydroxyethyl) uracil followed by oxidation, dealkylation, and transformation to the resulting sodium polysalt. The final polymer ($\bar M_n \approx 10^4 $) as well as the intermediate products were characterized by 1H-, 13C-, and 31P-NMR spectroscopy. 相似文献
3.
Noureddine Raouafi Khaled Boujlel Mohamed Lamine Benkhoud 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2471-2482
N-(-1H-Benzimidazol-2-yl) imidates 1a–c react with chlorophosphoramide to give the N-[-1-N,N,N′,N′-tetramethylphosphoramidoyl-1H-benzimidazol-2-yl]-imidates 2a–c or with dichlorophosphoramide to yield the bis[(N-1-benzimidazol-2-yl)-imidate] phosphoramide derivatives 3a–b. The reaction of compounds 2a–c toward primary amines is studied. The obtained amidine derivatives 4a–b were unambiguously characterized by different spectroscopic techniques (IR, 1H, 13C, and 31P NMR, and in some cases MS). 相似文献
4.
Li He Jin-Ping Zeng Da-Hai Yu Hang Cong Yun-Qian Zhang Qian-Jiang Zhu 《Supramolecular chemistry》2013,25(10):619-628
The host–guest interaction of symmetrical α,α′,δ,δ′-tetramethyl-cucurbit[6]uril (TMeQ[6]) with the hydrochloride salts of N,N′-bis(4-pyridylmethyl)-1,6-hexanediamine (P6), N,N′-bis(3-pyridyl-methyl)-1,6-hexanediamine (M6) and N,N′-bis(2-pyridylmethyl)-1,6-hexanediamine (O6) was investigated via single crystal X-ray diffraction, 1H NMR spectroscopy, electronic absorption spectroscopy and fluorescence spectroscopy. Single crystal X-ray diffraction showed that the hexyl moiety of P6 or M6 was incorporated in the cavity of TMeQ[6], while the two pyridylmethyl moieties of O6 were incorporated in the TMeQ[6] cavity in the solid state. The 1H NMR results in aqueous solution revealed that the TMeQ[6]-P6 and TMeQ[6]-M6 host–guest interaction systems produce a kinetic dumbbell-shaped inclusion complex at the initial stage and then an equilibrium pseudorotaxane-shaped inclusion complex as the only product after heating. However, only the pseudorotaxane-shaped inclusion complex was observed for the TMeQ[6]-O6 host–guest interaction system. Aqueous absorption spectrophotometric analysis showed that the dumbbell-shaped inclusion complexes were stable at pH 5.6, had a host–guest ratio of 2:1 and formed quantitatively at ~1011 l2/mol2 for the TMeQ[6]-M6 and TMeQ[6]-O6 systems. The transformation from dumbbell to pseudorotaxane-shaped inclusion complexes for the TMeQ[6]-P6 and TMeQ[6]-M6 host–guest systems yielded activation energies of 59.35 ± 1.55 and 78.7 ± 3.45 kJ/mol, respectively. The pseudorotaxane-shaped inclusion complexes were stable at pH 5.6, had a host–guest ratio of 1:1 and formed quantitatively at ~107 l/mol for the TMeQ[6]-M6 and TMeQ[6]-P6 systems. 相似文献
5.
Rhushirajeshwari M. Chalke 《高分子科学杂志,A辑:纯化学与应用化学》2017,54(9):556-564
Alkoxy substituted spirobifluorene derivatives namely 2,2′,7,7′-tetrabromo-3,6-bis(methoxy)-9,9′spirobifluorene (MSBF), 2,2′,7,7′-tetrabromo-3,6-bis(ethoxy)-9,9′spirobifluorene (ESBF), 2,2′,7,7′-tetrabromo-3,6-bis(butoxy)-9,9′spirobifluorene (BSBF), 2,2′,7,7′-tetrabromo-3,3′,6,6′-tetra(methoxy)-9,9′-spiro-9-silabifluorene (MSSiBF) and their key intermediates have been synthesised successfully. All compounds have been fully characterised by 1H and 13C NMR, FTIR, UV-visible spectroscopy, MS spectrometry. TGA analysis revealed good thermal stability. The systematic investigation on the solubility, thermostability and photophysical property of synthesized compound showed that alkoxy substituted spirobifluorene were unique in rigidity and have wide range of applications in molecular electronics and can be used as building units for optoelectronics material. 相似文献
6.
《Journal of Coordination Chemistry》2012,65(19):3391-3401
Two BiBr3 supramolecular complexes, [Bi(2-bpmp)Br2.06Cl0.94] (1) and [Bi(4-H2bpmp)Br4.29Cl0.71]·H2O (2) {2-bpmp = N,N′-bis(2-pyridylmethyl)piperazine and 4-bpmp = N,N′-bis(4-pyridylmethyl)piperazine}, were prepared by reaction of bismuth(III) chloride and potassium bromide with two nitrogen donor ligands under thermal gradient conditions using the branched tube method. Compounds 1 and 2 were structurally characterized by single-crystal X-ray diffraction. In monomeric 1, bismuth is coordinated by two pyridyl and piperazine nitrogens of 2-bpmp, and by three halides. Compound 2 is also monomeric but is bonded to only one pyridyl nitrogen. In both compounds, extensive hydrogen-bonding interactions lead to supramolecular networks; in 2, the hydrogen bonds are augmented by π–π stacking interactions. Thermal stabilities of both compounds were studied by thermal gravimetric and differential thermal analyses. Thermal decomposition of nanosized 1 and 2 in air produced BiOBr nanoparticles. 相似文献
7.
《Journal of Coordination Chemistry》2012,65(16):1807-1811
The complexes [M(CO)4(η2-H2L)] [M?=?Cr; 1, Mo; 2, W; 3] have been synthesized by photochemical reactions of VIB metal carbonyls [M(CO)6] [M?=?Cr,?Mo,?W] with N,N′-bis(salicylidene)-1,2-bis-(o-aminophenoxy)ethane (H2L) in THF and characterized by elemental analyses, FTIR, 1H?NMR and mass spectra. The H2L ligand is coordinated to the central metal as a bidentate ligand via the central azomethine nitrogen atoms in 1–3. 相似文献
8.
N. K. De Vries H. M. Buck 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4):267-279
Abstract A MNDO and 300-MHz 1H NMR study of some trigonal-bipyramidal (TBP) five-coördinated phosphorus (Pv) compounds is reported. It is shown by the MNDO calculations that, in the oxaphosphole Pv TBP compounds 5a-c, the electron distribution in the axial bonds of the TBP is affected by the electronegativity of the substituent at C4 of the oxaphosphole ring. With increasing electronegativity of the substituent at C4, the electron density on the axial exocyclic oxygen atom O1 decreases whereas the electron density on the axial endocyclic atom O1 increases. This is supported by a 1H NMR conformational analysis of the C1[sbnd]C2 bond of the oxaphosphole Pv TBP compounds 6–11. The gauche(-) rotamer fraction (O1 and O1 trans situated) of these compounds, which is correlated to the electron density on O1, is reduced to 30% as compared to the absolute axial g?rotamer fraction (59%) of the dioxaphosphole Pv TBP compound 13, most likely because of the presence of the carbonyl group at C4 of the oxaphosphole ring. So, both the 1H NMR and MNDO study show that electron withdrawing substituents on the oxaphosphole ring of Pv TBP compounds reverse the electron transfer in the axial P[sbnd]O bonds of the TBP (as compared to dioxaphosphole compounds), from exocyclic O1 towards endocyclic O1. 相似文献
9.
Max Herberhold Silke Gerstmann Und Bernd Wrackmeyer 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):273-283
Abstract Reactions of the salts K2SN2 and K[(NSN)R] (R = ′Bu, SiMe3 and P′Bu2) with organoelement chlorides R′R′ěl have been used to prepare four series of model sulfur diimides: R′R″E(NSN)ER″R′, ′Bu(NSN)ER″R′, Me3Si(NSN)E″R′ and tBu2P(NSN)ER″R′, respectively (E = C, Si, Ge, Sn; R′ and R″ = alkyl or aryl group). All compounds have been characterized by ′H and 13C NMR and—if possible—by 31P, 29Si and 119Sn NMR spectroscopy. The configuration (Z or E) of the substituents R and E″R′ has been assigned in several cases using tBu(NSN)tBu (1) as a reference. The E,Z assignment of 1H, 13C and 15N nuclei in 1 is based on selectively 1H-decoupled refocused INEPT 15N NMR and two-dimensional (2D) 13C/1H heteronuclear shift correlations. The sulfur diimides under study are in general fluxional in solution. 相似文献
10.
S. G. Peeran G. Hanumantha Reddy 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):9-22
Abstract The synthesis of (E)- and (Z)-1.2-bis(p-fluorophenylsulphenyl)stilbenes (2a and 2b) and 1,2-bis(p-fluorophenylsulphonyl)stilbenes (3a and 3b) was carried out and their configurations were consistent with their stereospecific synthesis. The isomeric 1,1-bis(p-fluorophenylsulphenyl)- and 1,1-bis(p-fluorophenylsulphonyl)-2,2-bis(phenyl)ethylenes (8 and 9) were also synthesised and configurations were established by degradative oxidation. Mass spectral rearrangements of all these compounds were examined. Mass spectra of 1,1-bis-sulphide and 1,1-bis-sulphone bears close relationship with those of (E)- and (Z)-isomeric counterparts. Smiles-type rearrangement observed in 1,2-bis-sulphides was absent in 1,2-bis-sulphones. McLafferty-type rearrangement involving hydrogen migration, from aryl group was noticed in both bis-sulphides and bis-sulphones. Vinyl migration to the sulphone oxygen predominates over aryl migration in three isomeric bis-sulphones. 相似文献
11.
Salma Moosun John A. Joule Minu G. Bhowon Sabina Jhaumeer-Laulloo 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):1383-1400
Abstract A series of novel acyclic and cyclic diaryl sulphides was synthesized from 2,2′-dithiobenzoic acid. The various diaryl sulphides were characterized by use of spectral (IR, 1H and 13C NMR, ESI/MS) and elemental analyses. The antimicrobial activities of the compounds were evaluated in terms of their minimum inhibition concentration (MIC) against a panel of clinical isolates bacteria and were found to possess only moderate antimicrobial activities. N,N′-Bis(2-hydroxyphenyl)-2,2′-thiodibenzamide (13), exhibiting a hydroxy group at the phenyl ring, was the most active antimicrobial agent within the series, with MIC values of 0.05 mg mL–1 and 10 mg mL–1 against Staphylococcus aureus and Bacillus cereus, respectively. The antioxidant efficiency of the diaryl sulphides was determined by 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging activity with 13 being the most active compound. The interaction of 2,2′-thiodibenzanilide, N,N′-bis(2-methylphenyl)-2,2′-thiodibenzamide, and N,N′-bis(2-hydroxyphenyl)-2,2′-thiobenzamide with guanine, glutamic acid, and urea were studied quantitatively with binding constants ranging from 1 × 103 M?1 to 2.7 × 104 M?1. 相似文献
12.
M. Chakrabarty A. Batabyal M. S. Morales-Ríos P. Joseph-Nathan 《Monatshefte für Chemie / Chemical Monthly》1995,126(6-7):789-794
Summary Unambiguous1H and13C NMR assignments for 4(3H)-quinazolinones1–6 and their corresponding 4-thiones7–12 have been made. This resulted in the revision of the previous assignments for the two benzenoid carbons (C-5 and C-8) of quinazolinones1,2,4, and5. Thionation of the nucleophilic amides1–6 has been found to cause a distinct change in the13C chemical shift of particularly C-4, but also of those of C-4a, C-5, and C-8a. One-bond and several long range heteronuclear coupling constants for the compounds have also been measured.
Kernresonanzspektroskopie von 4(3H)-Chinazolinonen und 4(3H)-Chinazolinthionen
Zusammenfassung Die1H- und13C-NMR-Spektren der 4(3H)-Chinazolinone1–6 und ihrer entsprechenden 4-Thione7–12 wurden zugeordnet. Dabei zeigte sich, daß eine frühere Zuordnung der beiden benzoiden Kohlenstoffe (C-5 und C-8) der Chinazolinone1,2,4 und5 falsch war. Ersatz des Sauerstoffs durch Schwefel in den nukleophilen Amiden1–6 führt insbesondere für C-4, aber auch für C-4a, C-5 und C-8a zu einer deutlichen Änderung der chemischen Verschiebung. Heteronukleare Kopplungskonstanten über eine und über mehrere Bindungen wurden bestimmt.相似文献
13.
《Journal of Coordination Chemistry》2012,65(16-18):2569-2583
AbstractTwo copper(II) coordination complexes, formulated as [Cu(tmen)(Clba)2] (1) and [Cu(tmen)(Hsal)2·H2O] (2) (where tmen?=?N,N,N′,N′-tetramethyl ethylenediamine (C6H16N2), Clba1? = 2-chlorobenzoate (C7H4ClO21?), and Hsal1? (C7H5O31? = monoanion of o-hydroxybenzoic acid (salicylic acid)), have been synthesized and characterized by elemental combustion analysis, spectroscopic techniques, thermal studies, and single crystal X-ray analyses. Complex 1 consists of two distinct monomeric units in which the coordination environment around the central copper(II) ion is a distorted octahedron with a CuN2O4 chromophore, constituted by a chelating tmen molecule, and two 2-chlorobenzoate1? anions coordinated through their carboxylate-O atoms in an asymmetrical bidentate fashion. Complex 2 is also a monomer and consists of an CuN2O3 chromophore, in which tmen is coordinated to Cu(II) through its two N atoms in a chelating bidentate fashion, and an aqua-O and the two o-hydroxybenzoate1? (HSal1?) anions are coordinated through one of their carboxylate-O atoms in a monodentate mode, forming a square pyramidal structure. Hydrogen bonding interactions especially of O–H…O, N–H…O, and C–H…Cl types interweave monomeric units and stabilize the overall crystal structures in both complexes. Thermal analysis and antibacterial activities of 1 and 2 against various bacterial strains were also investigated. 相似文献
14.
Synthesis and characterization of new copperphthalocyanine carrying mixed donor macrocyclic moieties
《Journal of Coordination Chemistry》2012,65(15):1667-1673
The new phthalocyanine peripherally substituted with a twelve-membered dioxadiaza macrocycle was synthesized by cyclotetramerization of 1,2-bis(2-{4′-[(4′-methylphenyl)-sulphonyl]-1′,7′-dioxa-4′,10′-diazacyclododecane})-4,5-dicyanobenzene (4) which was obtained from 1,2-bis(2-{4′-[(4′-methylphenyl)sulphonyl]-1′,7′-dioxa-4′,10′-diazacyclododecane})-4,5-dibromobenzene (3). Metallophthalocyanine was also prepared by the reaction of the dicyano-substituted macrocycle in the presence of anhydrous CuCN. The new compounds were characterized by a combination of elemental analysis, 1H and 13C?NMR, IR, electronic and mass spectroscopies. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(24):4389-4396
Solvothermal reactions of terphenyl-2,5,2′,5′-tetracarboxylic acid (H4qptc) and MII (M = Mn, Fe) in the presence of 1,2-bis(diphenylphosphino)ethane (dppe) afford two new coordination polymers, [M(qptc)(dppe-O)] n (M?=?Mn (1), Fe (2)) (1,2-bis(diphenylphosphoryl)ethane?=?dppe-O). The structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR, TGA, and magnetism. The MII in 1 and 2 are linked by qptc4? to form 2-D layers, which are further connected via the oxidized dppe (dppe-O) exhibiting a (4,6)-connected network with the (54.62)(510.63.7.8) topology. 相似文献
16.
《Journal of Coordination Chemistry》2012,65(18):2039-2045
New zinc(II) and mercury(II) complexes of 2,2′-diamino-4,4′-bis(1,3-thiazole) (DABTZ), [M(DABTZ)(CH3COO)2], have been synthesized and characterized by elemental analysis, IR-, 1H NMR-, 13C NMR spectroscopy and studied by thermal analysis and X-ray crystallography. The structural characterization of the [Zn(DABTZ)(CH3COO)2] complex shows the complex to be a monomer and the Zn coordinated by two nitrogen atoms of the “DABTZ” ligand and four oxygen atoms of the acetate anions. 相似文献
17.
《Journal of Coordination Chemistry》2012,65(19):3168-3178
Na[YbIII(Cydta)(H2O)2] · 5H2O (1) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and [YbIII(Hegta)] · 2H2O (2) (H4egta = ethyleneglycol-bis-(2-aminoethylether)-N,N,N′,N′-tetraacetic acid) were prepared and their composition and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques. Complex 1 crystallized in the triclinic crystal system with space group P 1; the YbIII is eight-coordinate by a hexadentate Cydta and two water molecules. Complex 2 is a protonated egta complex, crystallized in the monoclinic crystal system with space group P 2 1 /c; YbIII is coordinated only by the octadentate Hegta ligand. Both these complexes adopt a pseudo-square antiprismatic conformation. 相似文献
18.
Mononuclear Co(II), Zn(II) and Cd(II) complexes derived from bidentate or tridentate N,N′,N-bis((1H-pyrazol-1-yl)methyl)amines (Ln = LA, LB), where LA is N,N-bis((1H-pyrazol-1-yl)methyl)-3-methoxypropan-1-amine and LB is 3-methoxy-N,N-bis((3,5-dimethyl-1H-pyrazol-1-yl)methyl)propan-1-amine, have been synthesized and characterized. The geometry at Co(II) and Cd(II) for [LACoCl2], [LBCoCl2] and [LBCdBr2] with N,N′,N-tridentate ligands (Ln = LA, LB) can be described as a distorted trigonal bipyramid achieved by coordinative interaction of Npyrazole, two halides and the nitrogen of amine moiety. However, the molecular structure of four-coordinate [LAZnCl2] can be best described as tetrahedral, resulting in an eight-membered chelate ring. [LACoCl2] polymerized methyl methacrylate in the presence of modified methylaluminoxane at 60 °C and resulted in poly(methylmethacrylate) (PMMA) with higher molecular weight and narrower polydispersity index compared to the other synthesized complexes. However, all the synthesized complexes yielded syndiospecific PMMA, characterized using 1H NMR spectroscopy, with ca. 0.70. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(2):201-206
Three silver(I) complexes, [Ag(ca2en)(PPh3)]ClO4 (1), [Ag(ca2en)(PPh3)2]ClO4 (2) and [Ag(ca2en)2]ClO4 (3), where ca2en?=?N,N′-bis(trans-cinnamaldehyde)ethylenediimine, have been synthesized and characterized spectroscopically. The crystal structure of (1) was determined by X-ray diffraction methods. Crystal data for 1: C38H35AgClN2O4P, triclinic, P 1, a?=?12.086(2), b?=?18.204(2), c?=?8.550(2) Å, α?=?102.69(1), β?=?105.85(1), γ?=?91.47(1)°, V?=?1758.0(5) Å3, Z?=?2, R(F)?=?0.070, wR (F)?=?0.064, T?=?296?K. The coordination geometry of the Ag atom is distorted trigonal involving two N atoms of ca2en and one P atom of triphenylphosphine (PPh3). 相似文献
20.
《Journal of Coordination Chemistry》2012,65(4):269-280
Abstract The reactions of N′-2-hydroxyphenyl-6-methylpyridine-2-carbaldimine (LH) with tin(IV) chloride and organotin(IV) chlorides result in the formation of the corresponding tin(IV) and organotin(IV) complexes in which LH behaves as a uninegative tridentate ligand coordinating to the central tin atom via an N,N,O donor set. Crystal structure determinations of two of the compounds, n-butyldichloro[N′-2-hydroxyphenyl-6-methylpyridine-2-carbaldiminato(l-)N,N′,O]-tin(IV) (BuSnCl2.L) and diphenylchloro[N′-2-hydroxyphenyl-6-methylpyridine-2-carbaldiminato(l-)N,N′,O]tin(IV) (Ph2SnCl.L), have been performed and both structures feature distorted octahedral geometries about the tin centres. Systematic differences in the Sn-ligand separations are rationalised in terms of the reduced Lewis acidity of tin in Ph2SnCl.L. 相似文献