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1.
Two new isoprenylated benzofuran 3-ones, airlanggin A (1) and B (2) along with two known xanthones, ananixanthone (3) and trapezifolixanthone (4) were isolated from the stem bark of Calophyllum soulattri. Structures of all the compounds were elucidated using extensive spectroscopic methods, including UV, IR, HRESIMS, 1D and 2D NMR. Compounds 14 were evaluated for their cytotoxicity against P-388 cells, showing that compound 3 was the most active with IC50 0.68 μg/mL and compound 1 showed moderate activity with IC50 5.80 μg/mL.  相似文献   

2.
A simple and short approach for the synthesis of pyrazolo[3,4-b]quinoline (3a3p) and pyrazolo[4,3-c]quinoline (6a6 h) using various Lewis acid catalysts was developed. InCl3 was found to be more effective in providing greater yield of products compared to Yb(OTf)3, Sc(OTf)3, SnCl4, AlCl3, TiCl4, ZnCl2, FeCl3, and BF3 · Et2O. Moreover, a comparison of conventional and microwave methods has revealed that the latter method is more efficient compared to former one. Structures were confirmed by Fourier transform infrared, mass spectrometry, 1H and 13C NMR, X-ray crystallography, and elemental analyses. All of the synthesized compounds were evaluated for α-glucosidase inhibitory activity. Compounds 3a, 3p, 3i, 3 h, 3k, 3o, and 3 g exhibited anti α-glucosidase inhibitory activity with IC50 values of 57.5, 60.3, 65.9, 71.9, 80.8, 123.7, and 126.4 µM, respectively, which is quite comparable to the standard drug acarbose (IC50 = 115.8 µM).  相似文献   

3.
New nanocomposites, including different loading levels of sandwich-type polyoxometalates [(HOSnIVOH)3(XW9O34)2]n? (X = As (1), P (2) n = 12 and Si (3) n = 14) on Nd-doped TiO2 nanoparticles were prepared by a simple impregnation method. The nanocomposites were characterized by X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FTIR), and energy-dispersive X-ray spectroscopy. Compounds 13 were successfully loaded on Nd-doped crystallized anatase-phase TiO2 nanoparticles of 20–25 nm. Catalytic activities of nanocomposites were examined by carrying out the oxidation of sulfides and alcohols with H2O2. Simple synthesis method, reusability, and low amounts of the heterogeneous catalysts with a slight excess of H2O2 and mild reaction conditions make these oxidation reactions an environmentally benign chemical process.  相似文献   

4.
Both [Cu(DAT)2(PA)2] (1) and [Cu(DAT)2(HTNR)2] (2) were prepared from 1,5-diaminotetrazole (DAT) and copper trinitrophenol, 1 for picrate (PA) and 2 for styphnate acid (2,4,6-trinitro resorcinol, TNR), and were characterized by elemental analysis, FT-IR spectroscopy, and single crystal X-ray diffraction. The space group of these compounds is P21/c (monoclinic). The lattice parameters are similar [a = 11.405(3) Å, b = 14.867(3) Å, c = 8.099(2) Å for 1 and a = 12.262(3) Å, b = 14.900(3) Å, c = 7.243(2) Å for 2], except the β = 106.257(3)° in 1 and β = 92.989(4)° in 2. Both have extended structures due to hydrogen bonds, but there are some differences because of the ligands induced effect. Differential scanning calorimetry analysis shows that two exothermic processes take place in both complexes, the first peak temperatures are 488.2 K for 1 and 519.2 K for 2. The kinetic parameters of the first exothermic process were studied by using Kissinger’s method and Ozawa’s method, in which the enthalpy of formation (?7346 and ?5706 kJ M?1), critical temperature of thermal explosion (475.0 and 515.8 K), entropy of activation (ΔS), enthalpy of activation (ΔH), and free energy of activation (ΔG) were calculated and obtained as ?117.25 J K?1 M?1, 140.64 kJ M?1, 196.44 kJ M?1 and ?219.1 J K?1 M?1, 383.56 kJ M?1, 495.34 kJ M?1 for 1 and 2, respectively. The sensitivity test results showed that both compounds were sensitive to impact (<5 J) and flame (>20 cm) rather than friction.  相似文献   

5.
New ruthenium(II) complexes containing labile nitrile ligands have been prepared by treatment of either the polymer [{RuCl2(COD)}x] (COD = cycloocta-1,5-diene) (1) or its derivative [RuCl2(COD)(NCCH3)2]·NCCH3 (2) with the appropriate nitrile ligands in refluxing acetonitrile under argon. A new route to synthesis of trans-dichlorotetrakis(diphenylphosphine)ruthenium(II) (7) was also reported. A redetermination of the structure of 7 was undertaken and X-ray crystallographic data revealed that the complex crystallizes in the triclinic space group P-1 with unit cell dimensions a = 12.7016(9) Å, b = 13.0847(10) Å, c = 14.1498(10) Å, α = 101.46(3)°, V = 2080.6(3) Å3, Z = 2 and R = 0.0309. Its polymorph 7′ was also obtained. The crystal structure of 4 was also determined. This complex crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 27.0510(3) Å, b = 11.0984(13) Å, c = 13.0450(16) Å, α = 90°, V = 3886.5(8) Å3, Z = 8 and R = 0.0282.  相似文献   

6.
The rates of aqua substitution from [Pt{2-(pyrazol-1-ylmethyl)quinoline}(H2O)2](ClO4)2, [Pt(H2Qn)], [Pt{2-(3,5-dimethylpyrazol-1-ylmethyl)quinoline}(H2O)2](ClO4)2, [Pt(dCH3Qn)], [Pt{2-[(3,5-bis(trifluoromethyl)pyrazol-1-ylmethyl]quinoline}(H2O)2](ClO4)2, [Pt(dCF3Qn)], and [Pt{2-[(3,5-bis(trifluoromethyl)pyrazol-1-ylmethyl]pyridine}(H2O)2](ClO4)2, [Pt(dCF3Py)], with three sulfur donor nucleophiles were studied. The reactions were followed under pseudo-first-order conditions as a function of nucleophile concentration and temperature using a stopped-flow analyzer and UV/visible spectrophotometry. The substitution reactions proceeded sequentially. The second-order rate constants for substituting the aqua ligands in the first substitution step increased in the order Pt(dCH3Qn) < Pt(dCF3Qn) < Pt(H2Qn) < Pt(dCF3Py), while that of the second substitution step was Pt(dCH3Qn) < Pt(dCF3Qn) < Pt(dCF3Py) < Pt(H2Qn). The reactivity trends confirm that the quinoline substructure in the (pyrazolylmethyl)quinoline ligands acts as an apparent donor of electron density toward the metal center rather than being a π-acceptor. Measured pKa values from spectrophotometric acid–base titrations were Pt(H2Qn) (pKa1 = 4.56; pKa2 = 6.32), Pt(dCH3Qn) (pKa1 = 4.88; pKa2 = 6.31), Pt(dCF3Qn) (pKa1 = 4.07; pKa2 = 6.35), and Pt(dCF3Py) (pKa1 = 4.76; pKa2 = 6.27). The activation parameters from the temperature dependence of the second-order rate constants support an associative mechanism of substitution.  相似文献   

7.
Two new doubly methoxido-bridged MnIII dinuclear complexes, [MnIII(mphp)(μ-OCH3)(CH3OH)]2·2CH3OH (1) and ([MnIII(ahbz)(μ-OCH3)(CH3OH)]2·2CH3OH (2), have been synthesized by using the tridentate ligands H2mphp (H2mphp = 2-methyl-6-(pyrimidin-2-yl-hydrazonomethyl)-phenol) and H2ahbz (H2ahbz = N-(2-amino-propyl)-2-hydroxy-benzamide). The complexes have been characterized by single-crystal X-ray diffraction analysis and magnetic measurements. Complexes 1 and 2 have a similar dimeric molecular structure. Two [Mn(L)(CH3OH)]+ moieties (L2? = mphp2? or ahbz2?) are bridged by two μ-OCH3? groups in the axial-equatorial asymmetric manner. The coordination geometry of MnIII is an axially elongated octahedron with two oxygens of a methanol ligand and a methoxido ligand situated at the axial positions. Magnetic measurements indicate that 1 and 2 exhibit antiferromagnetic behavior with the fitting parameter of J = ?1.49(3) cm?1, D = ?1.3(1) cm?1, g = 1.98(1) and zJ′ = ?0.18(4) cm?1 for 1, and J = ?1.6(2) cm?1, D = 4.5(3) cm?1, g = 2.06(1) and zJ′ = 1.4(1) cm?1 for 2 on the basis of the spin Hamiltonian ? = ?2J?Mn1?Mn2.  相似文献   

8.
A series of LnIII–SrII heterometallic coordination polymers formulated as [Ln2Sr3(pda)6(H2O)18]·nH2O (Ln = Pr-1, n = 14; Nd-2, n = 12; Sm-3, n = 11; Eu-4, n = 11; Gd-5, n = 16; Tb-6, n = 13; Dy-7, n = 13) were synthesized via assembly of Ln(NO3)3·6H2O, SrCl2·6H2O, pyridine-2,6-dicarboxylic acid (H2pda) and imidazole (im) in H2O/C2H5OH solution. Single crystal X-ray diffraction revealed that they are isostructural. All of these complexes possess ladder-shaped 1-D chain structures. The luminescent properties of Sm-3, Eu-4, Gd-5, Tb-6 and Dy-7 have been investigated. The solid-state quantum yields and the lifetimes of Eu-4 and Tb-6 are also studied.  相似文献   

9.
Two tetranuclear nickel(II) complexes, [Ni4 (p-BrPhHIDC)4(py)4(H2O)4]·CH3OH (p-BrPhH3IDC = 2-(p-bromophenyl)-1H-imidazole-4,5-dicarboxylic acid) (1) and [Ni4(p-ClPhHIDC)4 (CH3CN)4(H2O)4]·4H2O (p-ClPhH3IDC = 2-(p-chlorophenyl)-1H-imidazole-4,5-dicarboxylic acid, py = pyridine) (2), have been solvothermally synthesised and structurally characterised. Both compounds consist of similar tetranuclear Ni(II) cores, in which the imidazole dicarboxylate ligands adopt the similar coordination mode. The thermal properties of 1 and 2 have been investigated. Also, it is discovered that there exists antiferromagnetic coupling between the Ni(II) ions in 1 and 2; the best fittings to the experimental magnetic susceptibilities gave J = ? 9.89 cm? 1 and g = 2.18 for 1, and J = ? 10.54 cm? 1 and g = 2.14 for 2.  相似文献   

10.
《Analytical letters》2012,45(8):1148-1156
Abstract

A reverse-phase high-performance liquid-chromatographic photodiode array detection (DAD) method has been developed and validated for the simultaneous determination of five isoflavones in Millettia nitida var. hirsutissima: hirsutissimiside B, sphaerobioside, lanceolarin, formononetin, and afromosin. The method utilized a C18 column (4 µm, 250 × 4.6 mm) with an acetonitrile and aqueous H3PO4 gradient and ultraviolet detection at 259 nm. The recovery of the method is 94.1–105.9%, and linearity (r > 0.9996) is obtained for all the isoflavones.  相似文献   

11.
The crude extracts of tubers of Aconitum spicatum (Bruhl) Stapf were investigated for in vitro antileishmanial activity against Leishmania major. The dichloromethane extract at pH 2.5 showed antileishmanial activity with IC50 value of 27.10 ± 0.0 μg/mL. Chromatographic purification of the dichloromethane extract led to isolation of three C-19 norditerpenoid alkaloids indaconitine (1), chasmaconitine (2) and ludaconitine (3). Compounds 3 and 2 showed antileishmanial activity with IC50 = 36.10 ± 3.4 and 56.30 ± 2.1 μg/mL, respectively. Compound 1 was less effective (IC50 > 100 μg/mL). The cytotoxicity of compounds 1, 2 and 3 studied against MCF7, HeLa and PC3 cancer cell lines and 3T3 normal fibroblast cell line did not show cytotoxicity at 30 μM.  相似文献   

12.
Complexes of [Zn(ibup)2(4,4′-bipy)]n 1, [Zn(ibup)2(phen)] 2, [Zn(ibup)2(2,9-dmphen)] 3, [Zn(ibup)2(1,2-dmimidazole)2] 4, and [Zn(ibup)2(2-am-6-picoline)2] 5 (ibu = ibuprofen, 4,4′-bipy = 4,4′-bipypyridine, phen = 1,10-phenanthroline, 2,9-dmephen = 2,9-dimethyl-1,10-phenanthroline, 1,2-dmimidazole = 1,2-dimethylimidazole, and 2-am-6-picoline = 2-amino-6-picoline) were prepared and characterized. The crystal structure of 1 was determined by single-crystal X-ray diffraction. The in vitro anti-bacterial activities for the complexes against Gram-positive (Micrococcus luteus, Staphylococcus aureus and Bacillus subtilis) and Gram-negative (Escherichia coli, Klebsiella pneumonia and Proteus mirabilis) bacteria were done using the agar well-diffusion method. Complexes 13 showed anti-bacterial activity against Gram-positive bacteria, while 4 and 5 did not exhibit anti-bacterial activity. Complexes 2 and 3 were selected for further studies. Complexation of zinc-ibuprofen with phen as in 2 decreased the anti-bacterial activity against most of the bacteria used. The complexation in 3 decreased the anti-bacterial activity in Gram-positive bacteria but for Gram-negative bacteria, the overall anti-bacterial activity of uncoordinated 2,9-dmphen was enhanced upon coordination with zinc ibuprofen.  相似文献   

13.
Three Zn(II) complexes, [Zn2(bpp)2(FNA)2]·H2O (1), [Zn(bpp)(FNA)]·H2O (2), and Zn2(bpp)2(FNA)2 (3) (bpp = 1,3-bi(4-pyridyl)propane, H2FNA = 4-nitrobenzene-1,2-dicarboxylic acid), were synthesized and characterized by single-crystal and powder X-ray diffraction methods, IR spectroscopy, TG analyses, elemental analyses, and fluorescent analysis. In 1, the Zn(II) ions are linked by FNA anions and bpp into 2-D layers. The Zn(II) ions in 2 are bridged by FNA anions into chiral chains, which are interlinked by bpp into 3-D metal–organic framework with (65·8) CdS topology. Complex 3 features 1-D zigzag chains, which are interconnected by bpp ligands to give a 3-D framework with (6·74·8)(64·7·8) topology. Complexes 2 and 3 exhibit significant ferroelectric behavior (for 2 remnant polarization Pr = 0.050 μC cm?2, coercive field Ec = 1.13 kV cm?1, saturation of the spontaneous polarization Ps = 0.239 μC cm?2; for 3 Pr = 0.192 μC cm?2, Ec = 4.64 kV cm?1, Ps = 0.298 μC cm?2).  相似文献   

14.
Homo- and heteronuclear bimetallic carbene complexes of group VII transition metals (Mn and Re), with cymantrene or cyclopentadienyl rhenium tricarbonyl as the starting synthon, have been synthesized according to classic Fischer methodology. Crystal structures of the carbene complexes with general formula [RC5H4 M'(CO)2{C(OEt)(C5H4 M(CO)3)}], where M = M′ = Mn, R = H (1), R = Me (2); M = Mn, M′ = Re, R = H (3); M = M′ = Re, R = H (4); and M = Re, M′ = Mn, R = H (5), are reported. A density functional theory (DFT) study was undertaken to determine natural bonding orbitals (NBOs) and conformational as well as isomeric aspects of the binuclear complexes. Application of second-order perturbation theory (SOPT) of the NBO method revealed stabilizing interactions between the methylene C–H bonds and the carbonyl ligands of the carbene metal moiety. Energy calculations in the gas phase of the cis and trans conformations of the Cp rings relative to one another are comparable, with the trans conformation slightly lower in energy. The theoretical findings have also been confirmed with single-crystal X-ray diffraction, and all solid-state structures are found in the trans geometry.  相似文献   

15.
16.
Four novel Schiff base ligands and their copper(II) complexes, [Cu(L1)2] (1), [Cu(L2)2] (2), [Cu(L3)2] (3), and [Cu(L4)2] (4), were synthesized and characterized by elemental analyses, FT-IR, and UV–Vis spectroscopy. The ligands were synthesized from the condensation of 2-methoxyethylamine with various salicylaldehyde derivatives (x-salicylaldehyde for HLn, x = H (n = 1), 5-Br (n = 2), 3-OMe (n = 3), and 4-OMe (n = 4)). The molecular structures of 1, 2, and 3 were determined by the single crystal X-ray diffraction technique. The redox behavior studies of the complexes in acetonitrile display the electronic effects of the groups on the redox potential. The antioxidant activity of the Schiff base ligands and their Cu(II) complexes was evaluated using the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging method and FRAP assay. Furthermore, the in vitro anticancer activity of compounds was screened, including MTT and migration assays against gastric cancer cell line (MKN-45). The results show that all ligands and complexes have antioxidant and anticancer activity in a concentration-dependent way.  相似文献   

17.
The complexes [Zn(phenylacetato)2(2-aminopyridin)2] (3), [Zn(phenylacetato)2(1,10-phenanthroline)]·H2O (4), and [Zn(phenylacetato)2(2,9-dimethyl-1,10-phenanthroline)]·0.5 H2O (5) were prepared and characterized by IR-, UV–Visible, 1H and 13C NMR spectroscopy, and single crystal X-ray diffraction. BNPP hydrolysis of the complexes and their parent nitrogen ligands showed that the hydrolysis rate of bis-(4-nitrophenyl) phosphate (BNPP) was 1.7 × 105 L mol?1 s?1 for 3, 3.1 × 105 L mol?1 s?1 for 4 and 4.3 × 104 L mol?1 s?1 for 5. Antibacterial activities show the effect of complexation on activity against Gram-positive (S. epidermidis, S. aureus, E. faecalis, M. luteus and B. subtilis) and Gram-negative (K. pneumonia, E. coli, P. mirabilis and P. aeruginosa) bacteria using the agar well diffusion method. Complex 4 showed good activity against G? bacteria except P. aeruginosa, and against G+ bacteria except E. ferabis. Complex 5 showed no activity against G? bacteria, low activity against M. luteus and B. subtilis bacteria and high activity against S. epidemidis and S. aureus. Complex 3 did not show any activity against G? or G+ bacteria.  相似文献   

18.
Two iron(II) complexes, [FeII(pytBuN3)2](FeCl4) (1) and [FeII(pytBuMe2N3)Cl2] (2), with sterically constrained pytBuN3 and pytBuMe2N3 chelate ligands (pytBuN3 = 2,6-bis-(aldiimino)pyridyl; pytBuMe2N3 = 2,6-bis-(ketimino)pyridyl), have been synthesized and characterized by elemental analysis, IR, UV–vis spectra, and preliminary X-ray single-crystal diffraction. The latter revealed that Fe(II) in 1 is six-coordinate by six nitrogen donors from two bisiminopyridines in a distorted octahedron. Complex 2 reacts with thiourea with a second-order rate constant k2 = (2.50 ± 0.05) × 10?3 M?1 s?1 at 296 K, and the reaction seemed to be slow. In a similar way, the interaction of 2 and DNA was studied by fluorescence and absorption spectroscopy. The results revealed that 2 caused fluorescence quenching of DNA through a dynamic quenching procedure. The binding constants KA, Kapp, and KSV as well as the number of binding sites between 2 and DNA were determined.  相似文献   

19.
The phosphonium salts [Ph2P(CH2)nPPh2CH2C(O)C6H4-m-OMe]Br (n = 1 (S1) and n = 2 (S2)) were synthesized in the reaction of bis(diphenylphosphino)methane (dppm) and bis(diphenylphosphino)ethane (dppe) with 2-bromo-3?-methoxy acetophenone, respectively. Further treatment with NEt3 gave the phosphorus ylides Ph2P(CH2)nPPh2C(H)C(O)C6H4-m-OMe (n = 1 (Y1) and n = 2 (Y2)). These ligands were treated with [MCl2(cod)] (M = Pd or Pt; cod = 1,5-cyclooctadiene) to give the P, C-chelated complexes, [MCl2(Ph2P(CH2)nPPh2C(H)C(O)C6H4-m-OMe)] (n = 1, M = Pd (3), Pt (4), and n = 2, M = Pd (5), Pt (6)). These compounds were characterized by elemental analysis, spectroscopic methods, UV–visible, and fluorescence emission spectra. Further, the structures of complexes 3 and 6 were characterized crystallographically. The palladium complexes 3 and 5 proved to be excellent catalysts for the Suzuki reactions of various aryl chlorides. Also, a theoretical study on the structure of complexes 3–6 has been investigated at the BP86/def2-SVP level of theory. The strength and nature of donor?acceptor bonds between the phosphorus ylides (L) and MCl2 fragment in the [LMCl2] (M = Pd, Pt, L = Y1, Y2) were studied by NBO and energy decomposition analysis (EDA), as well as their natural orbitals for chemical valence variation (EDA-NOCV).  相似文献   

20.
Ethanol extract of the aerial parts of Bergenia ligulata was subjected to solvent–solvent separation followed by various chromatographic techniques that lead to isolation of bergenine (1), p-hydroxybenzoyl bergenin (2), 11-O-galloylbergenin (3) and methyl gallate (4) as major constituents. Ethyl acetate fraction showed a dose-dependent urease inhibitory pattern with IC50 value of 54μg/mL. Structures of compounds 1 and 3 were established by XRD and 2, 4 by NMR. All these compounds were subjected to DPPH scavenging activity, reducing power assay and urease inhibitory activity. The EC50 7.45 ± 0.2 μg/mL and 5.39 ± 0.28 μg/mL values in terms of antioxidant and reducing power, respectively, were less for 3. Compounds 13 showed moderate to significant urease inhibitory potential with IC50 57.1 ± 0.7, IC50 48.4 ± 0.3 and 38.6 ± 1.5. Antioxidant activities and urease inhibitory potential were investigated and compound 3 was found to be the most active.  相似文献   

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