共查询到20条相似文献,搜索用时 843 毫秒
1.
Jing-Jing Zhu Chao-Feng Zhang Mian Zhang S.W. Annie Bligh Li Yang Zhi-Min Wang Zheng-Tao Wang 《Journal of chromatography. A》2010,1217(33):5384-5388
Six C-glucosyl anthrones were characterized as three pairs of epimers by on-line high performance liquid chromatography–circular dichroism (HPLC–CD) analysis and isolated from the roots of Rumex dentatus by column chromatography. Their structures were elucidated by mass spectrometry, nuclear magnetic spectroscopy and HPLC–CD analysis. They are 10R-C-β-d-glucosyl-10-hydroxyemodin-9-anthrone (rumejaposide E, 1) and 10S-C-β-d-glucosyl-10-hydroxyemodin-9-anthrone (rumejaposide F, 2), 10R-C-β-d-glucosylemodin-9-anthrone (rumejaposide G, 3) and 10S-C-β-d-glucosylemodin-9-anthrone (rumejaposide H, 4), 10S-C-β-d-glucosyl-10-hydroxychrysophanol-9-anthrone (cassialoin, 5) and 10R-C-β-d-glucosyl-10-hydroxychrysophanol-9-anthrone (rumejaposide I, 6). Rumejaposides F–I (2–4 and 6) were new C-glucosyl anthrones. Rumejaposide E (1) and cassialoin (5) were isolated for the first time in Rumex plants. On-line HPLC–UV–CD analysis was a useful tool for structure elucidating epimeric C-glycosides anthrones 3–6 because of the poor stability of the pure isomers (3 and 4) and the minute quantity of 5 and 6 in the mixture. 相似文献
2.
Metal-free (2) and Co(II), Zn(II), Ni(II), Cu(II) metallophthalocyanines (2a–d) with four 4-phenyloxyacetic acid groups on the periphery were prepared by cyclotetramerization of new p-(3,4-dicyanophenoxy)phenylacetic acid (1) and the corresponding divalent metal salts. Further reactions of these products with thionylchloride and then benzylamine in tetrahydrofuran, and octanol in pyridine gave amide (3, 3a–d) and ester (4, 4a–d) derivatives, respectively. The new compounds have been characterized by elemental analyses, IR, UV–Vis, mass and 1H NMR spectroscopy. The redox properties of compounds 2 and 2a–d were identified by cyclic voltammetry. 相似文献
3.
The reaction of bromoalkanes (R–Br; (3), R=CnH2n+1, n=4 (a), 8 (b), 12 (c),18 (d)) and bromobenzyl derivatives (R′–Br; (4), R′=CH2C6H2(CH3)3-2,4,6 (a); CH2C6H(CH3)4-2,3,5,6 (b); CH2C6(CH3)5 (c)) with 1H-imidazo[4,5-f][1,10]-phenanthroline (IP)(L2) gave the corresponding 1-R-imidazo[4,5-f][1,10]-phenanthroline (IPR)(L3a–d) and 1-R′-imidazo[4,5-f][1,10]-phenanthroline(IPR')(L4a–c) ligands, respectively. Treatment of L3a–d and L4a–d with [Ru(p-cymene)Cl2]2 led to the formation of [Ru(p-cymene)(IPR)Cl]Cl (RuL3a–d) and [Ru(p-cymene)(IPR′)Cl]Cl (RuL4a–c). New ruthenium(II) complexes RuL3a–d and RuL4a–c were characterized by elemental analysis, FTIR, UV–visible and NMR spectroscopy. In order to understand effects of these changes on the N-substituent of imidazol on IP and how they translate to catalytic activity, these new RuL2, RuL3a–d and RuL4a–c were applied in the transfer hydrogenation of ketones by 2-propanol in presence of potassium hydroxide. The activities of the catalysts were monitored by NMR and GC analysis. 相似文献
4.
Diana Visinescu Luminita M. Toma Oscar Fabelo Catalina Ruiz-Pérez Francesc Lloret Miguel Julve 《Polyhedron》2009
The reaction of acetonitrile (1–5) and mixed acetonitrile/water 1:1 (6–9) solutions containing the cyanide-bearing [Fe(bipy)(CN)4]− building block (bipy = 2,2′-bipyridine) and the partially blocked [Ln(bpym)]3+ cation (Ln = lanthanide trivalent cation and bpym = 2,2′-bipyrimidine) has afforded two new families of 3d–4f supramolecular assemblies of formula [Ln(bpym)(NO3)2(H2O)3][Fe(bipy)(CN)4] · H2O · CH3CN [Ln = Sm (1), Gd (2), Tb (3), Dy (4) and Ho (5)] and [Ln(bpym)(NO3)2(H2O)4][Fe(bipy)(CN)4] [Ln = Pr (6), Nd (7), Sm (8), Gd (9)]. They crystallize in the P21/c (1–5) and P2/c (6–9) space groups and their structures are made up of [Fe(bipy)(CN)4]− anions (1–9) and [Ln(bpym)(NO3)2(H2O)n]+ cations [n = 3 (1–5) and 4 (6–9)] with uncoordinated water and acetonitrile molecules (1–5) which are interlinked through an extensive network of hydrogen bonds and π–π stacking into three-dimensional motifs. Both families have in common the occurrence of the low-spin iron(III) unit [Fe(bipy)(CN)4]− where two bipy–nitrogen and four cyanide–carbon atoms build a somewhat distorted octahedral surrounding around the iron atom [Fe–N = 1.980(3)–1.988(3) Å (1–5) and 1.988(2)–1.992(2) Å (6–9); Fe–C = 1.904(5)–1.952(4) Å (1–5) and 1.911(2)–1.948(3) Å (6–9)]. The main structural difference between both families concerns the environment of the lanthanide atom which is nine- (1–5)/10-coordinated (6–9) with a chelating bpym, two bidentate nitrate and three (1–5)/four (6–9) water molecules building distorted monocapped (1–5)/bicapped (6–9) square antiprisms. This different lanthanide environment is at the origin of the different hydrogen bonding pattern of the two families of compounds. 相似文献
5.
The novel tridentate chiral ligand 2,6-bis{[(1R,2S,4R)-2-hydroxy-1,3,3-trimethyl-bicyclo[2.2.1]hept-2-yl]}pyridine (1) was readily prepared by reaction of 2,6-dilithiopyridine with (R)-(−)-fenchone. Reaction of 1 with [MoO2(acac)2] resulted in the formation of the new metal-oxo five-coordinated complex [MoO2(ONO)] (2) [ONO = (1 – 2H)]. The reactivity of 2 has been studied and the derivatives [MoS2(ONO)] (3) and [MoO(O2)(ONO)] (4) were prepared. The compounds 1–4 have been characterised by 1H and 13C{1H} NMR, microanalysis and IR spectroscopy. Furthermore, the molecular structures of 1 and 2 have been determined by single-crystal X-ray diffraction. The behaviour of 2 as catalyst in oxotransfer and in nucleophilic substitution of propargylic alcohols reactions has been tested. 相似文献
6.
The reactions of Mo2(O2CCH3)4 with different equivalents of N,N′-bis(pyrimidine-2-yl)formamidine (HL1) and N-(2-pyrimidinyl)formamide (HL2) afforded dimolybdenum complexes of the types Mo2(O2CCH3)(L1)2(L2) (1) trans-Mo2(L1)2(L2)2 (2) cis-Mo2(L1)2(L2)2 (3) and Mo2(L2)4 (4). Their UV–Vis and NMR spectra have been recorded and their structures determined by X-ray crystallography. Complexes 2 and 3 establish the first pair of trans and cis forms of dimolybdenum complexes containing formamidinate ligands. The L1 ligands in 1–3 are bridged to the metal centers through two central amine nitrogen atoms, while the L2 ligands in 1–4 are bridged to the metal centers via one pyrimidyl nitrogen atom and the amine nitrogen atom. The Mo–Mo distances of complexes 1 [2.0951(17) Å], 2 [2.103(1) Å] and 3 [2.1017(3) Å], which contain both Mo?N and Mo?O axial interactions, are slightly longer than those of complex 4 [2.0826(12)–2.0866(10) Å] which has only Mo?O interactions. 相似文献
7.
Gannerla Saidachary Kasagani Veera PrasadMudulkar Sairam Bhimapaka China Raju 《Tetrahedron letters》2014
A facile method has been developed for the synthesis of 4H-chromene-3-carboxylates 3a–d by the nucleophilic substitution reaction of 2-hydroxy-2H-chromene-3-carboxylates 2a–d with triethylsilane in the presence of BF3·O(C2H5)2. Cyclocondensation of 4H-chromene-3-carboxylates 3a–d with benzylamines 4a–d afforded a series of 2,3-dihydrochromenopyrrolones 5a–p and with propargylamine afforded 2-propynyl-2,3-dihydrochromenopyrrolones 6a–d. Click reaction of 6a–d with benzyl azides 7a–d provided a series of 1H-1,2,3-triazolylmethyl-2,3-dihydrochromenopyrrolones 8a–p. Thus synthesized compounds 3a–d, 5a–p, 6a–d, and 8a–p are novel heterocyclic compounds and being reported for the first time. 相似文献
8.
A large number of novel N-aryl modified monocyclic γ-lactam derivatives have been prepared via Pd(0) catalyzed heteroarylation in the N-aryl part of (±) cis and (±) trans γ-lactam carboxylate derivatives 3(a–f) and 6(a–f), respectively, with furan-2-boronic acid and thiophen-2-boronic acid. (±) cis Methyl 1-(2-bromoaryl)-5-oxo-3-aryl/heteroarylpyrrolidin-2-carboxylate derivatives 3(a–f), were prepared in good yields from 1(a–f) via hydrolysis, stereoselective decarboxylation, followed by esterification. Corresponding trans isomers 6(a–f) were prepared by the standard method already reported by us. 相似文献
9.
Santosh Kurhade Vandana Rajopadhyay Satheesh Veerappa Avaragolla Summon Koul Parimi Atchuta Ramaiah Debnath Bhuniya 《Tetrahedron letters》2014
l-(N-Cbz)-7-azaisotryptophan, l-(N-Cbz)-1a, a new isostere of tryptophan, was synthesized by reacting Li2-(N-Boc)-2-amino-3-picoline, Li2-(N-Boc)-2a, with appropriately protected l-aspartic acid followed by simple functional group manipulation. This synthetic success led us to access a set of analogs of azaisotryptophan (4a–c; 6a–c) as well as a new class of chiral amines (7a–c; 8a–c) for future application in asymmetric synthesis and design of homochiral ligands. Further, we have generalized the method substantiating a variety of new azaindol-2-yl derivatives (10aa–10lc) with functionalized substituents. In a preliminary luminescence characterization, l-(N-Cbz)-1a has exhibited about 30 nm bathochromic shifted fluorescence emission compared to tryptophan and (N-Cbz)-tryptophan. 相似文献
10.
Biao Yang Guang-Ying Chen Xiao-Ping Song Liu-Qing Yang Chang-Ri Han Xiang-Yang Wu Cai-Juan Zheng Xu Ran Ri-Feng Tang 《Tetrahedron letters》2013
Phytochemical study of the twigs of Trigonostemon xyphophylloides led to the isolation of six new heterodimers, trigoxyphins O (1) and R–T (4–6) comprising of two different degraded diterpenoids, and trigoxyphins P (2) and Q (3) comprising a degraded diterpenoid and a phenylpropanoid, together with a known homodimer, neoboutomannin (7). The structures and relative configurations were elucidated on the basis of extensive spectroscopic analysis, including 1D and 2D NMR experiments. Compounds 1–6 were evaluated for their cytotoxicity against four human tumour cell lines by MTT assay. 相似文献
11.
The energetic nitrogen-rich compounds 1,3-bis(1-methyltetrazol-5-yl)triaz-1-ene (4) and 1,3-bis(2-methyltetrazol-5-yl)triaz-1-ene (5) were synthesized by diazotation of 1-methyl-5-aminotetrazole (2) and 2-methyl-5-aminotetrazole (3), respectively, by using half an equivalent of sodium nitrite. The reaction of 4 and 5 with diluted ammonia solution yields ammonium bis(1-methyltetrazol-5-yl)triazenate (6) and ammonium bis(2-methyl-tetrazol-5-yl)triazenate (7). Treating of 4 and 5 with aqueous sodium hydroxide solution yields sodium bis(1-methyltetrazol-5-yl)triazenate (8) and sodium bis(2-methyltetrazol-5-yl)triazenate (9) almost quantitative. Compounds 8 and 9 were methylated using methyl iodide and dimethyl sulfate, respectively, originating bis(1-methyltetrazol-5-yl)-3-methyltriaz-1-ene (10) and bis(2-methyltetrazol-5-yl)-3-methyltriaz-1-ene (11). The products 4–11 were characterized by Raman, IR, multinuclear NMR and UV–Vis spectroscopy, mass spectrometry, elemental analysis and differential scanning calorimetry. The structures of the crystalline state of 4 · H2O, 5, 8 · MeOH, 10 and magnesium bis(2-methyltetrazol-5-yl)triazenate (12) were determined by low temperature single crystal X-ray diffraction. The heats of formation ΔfH° of 4–7, 10 and 11 were calculated using energies of combustion ΔcU° determined by bomb calorimetry, resulting in strongly endothermic values. With these data and by using calculated (4, 5, 10) as well as measured (6, 7, 11) crystal densities, several detonation parameter (heats of explosion, detonation pressure, detonation velocity, explosion temperature) were calculated by the explo5 software. In addition, the specific impulse of different propellant mixtures of the most promising compound 6 with ammonium dinitramide (ADN) were computed. Furthermore the n-octanol/water partition coefficients of 4, 5, 6 and 7 were determined and the long-term stability of 6 was tested by thermal safety calorimetry. Lastly the sensitivities toward impact and friction as well as electrical discharge were determined by the BAM drophammer, friction tester and a small scale electrical discharge tester. 相似文献
12.
Jun-Wei He Zhen-Qiang Mu Hao Gao Guo-Dong Chen Qin Zhao Dan Hu Jing-Zu Sun Xiao-Xia Li Yan Li Xing-Zhong Liu Xin-Sheng Yao 《Tetrahedron》2014
Six new polyesters, talapolyesters A–F (1–4, 14, and 16), together with 11 known ones 15G256ν (5), 15G256ν-me (6), 15G256π (7), 15G256β-2 (8), 15G256α-2 (9), 15G256α-2-me (10), 15G256ι (11), 15G256β (12), 15G256α (13), 15G256α-1 (15), and 15G256ω (17), were isolated from the wetland soil-derived fungus Talaromyces flavus BYD07-13, and their structures were determined by NMR and MS spectroscopic data. Among them, 1–4 and 16 were assembled in a different manner from that of the known 256 polyesters. All the polyesters are composed of (R)-2,4-dihydroxy-6-(2-hydroxypropyl)benzoic acid and (R)-3-hydroxybutyric acid/(S)-3,4-dihydroxybutyric acid residues. The absolute configurations of the residues were determined by alkaline hydrolysis. The cytotoxicity against five tumor cell lines of these compounds was examined, and a tight structure–activity relationship is proposed. 相似文献
13.
Xinzhou Yang Chao Wang Jing Yang Dingrong Wan Qinxiong Lin Guangzhong Yang Zhinan Mei Yunjiang Feng 《Tetrahedron letters》2014
Two new eudesmane-type sesquiterpenes, 9α-hydroxycurcolonol (1) and 3α-hydroxy-4-deoxy-5-dehydrocurcolonol (2), along with nine known sesquiterpenes (3–11), were isolated from the roots of Chloranthus angustifolius. The antimicrobial activities of compounds 1–11 were evaluated against five bacteria and six fungal strains. Compounds 6–11 showed potent activities against Candida albicans with MIC values ranging from 4 to 8 μg/mL. The structures of the two new compounds 1 and 2 were established by a detailed analysis of their NMR and mass spectroscopic data. 相似文献
14.
The complexes [Co(N^O)2] (1) and [Cu(N^O)2] (2) {N^O = η2-(N,O) coordinated 2-pyrazinecarboxylic acid} have been synthesized and characterized by elemental (including metal) analyses, FT-IR spectroscopy and powder X-ray diffraction. The molecular structure of complex 2 was determined by single X-ray crystallography. In the molecule, the Cu atom occupies the center of a square planar geometry, which consists of two trans-O atoms and two trans-N atoms of two 2-pyrazinecarboxylic acid ligands. The complexes 1 and 2 were well encapsulated into zeolite–Y super-cage to yield the corresponding zeolite–Y encapsulated metal complexes, abbreviated herein as [Co(N^O)2]–Y (3) and [Cu(N^O)2]–Y (4). Similarly, the metal complexes 1 and 2 were immobilized on alumina and organically modified silica surfaces to lead to the formation of immobilized metal complexes [Co(N^O)2]–Al2O3 (5); [Cu(N^O)2]–Al2O3 (6); [Co(N^O)2]–AMPS (7) and [Cu(N^O)2]–AMPS (8) (AMPS = aminopropyl silica). Elemental (including metal) analyses, FT-IR spectroscopy, powder X-ray diffraction and thermal analysis have been used to characterize these materials. The catalytic activity of all the catalysts 1–8 towards the oxidation of cyclohexene into different chemically and pharmaceutically important products were evaluated under homogeneous and heterogeneous conditions. In order to obtain a maximum conversion of cyclohexene, the reaction parameters, like reaction temperature and time, were optimized. Under the optimized conditions, a maximum of 90.47% cyclohexene conversion was achieved with [Cu(N^O)2]–Y (4) with a 1:2 molar ratio reaction of cyclohexene and H2O2. 相似文献
15.
Mariko Kitajima Minako Anbe Noriyuki Kogure Sumphan Wongseripipatana Hiromitsu Takayama 《Tetrahedron》2014
Seven new indole alkaloids (aspidofractinine type 1–3, kopsine type 5, strychnos type 6, and vincamine type 7, 8) were isolated from Kopsia jasminiflora (Apocynaceae) collected in Thailand. 5-Oxokopsinic acid (4) was isolated from nature for the first time. The structures of the new alkaloids were determined by spectroscopic analyses and chemical transformation of a known alkaloid. 5,6-Secokopsinine (1) possesses a dialdehyde function that is formed by oxidative cleavage of the C-5–C-6 bond of kopsinine (9). New vincamine-type alkaloid 8 showed potent inhibitory activity toward human cancer cell lines (A549, HT29, HCT116). 相似文献
16.
Three new cyclic hexapeptides, designated as rubischumanins A–C (1–3), together with three known ones (4–6) were isolated from the roots and rhizomes of Rubia schumanniana. The structures were elucidated on the basis of extensive spectroscopic analysis. Cytotoxicity of these compounds was evaluated and compounds 1, 2, 4, and 5 showed cytotoxicity against A549, BGC-823, and Hela cell lines. 相似文献
17.
Jokin Carrillo Alex GómezAnna M. Costa Patricia Fernández Carles IsartMireia Sidera Jaume Vilarrasa 《Tetrahedron letters》2014
The esterification of fragment C1–C8 (2) with fragment C16–C23 (3) to give iodo derivative 4, followed by a Pd-catalysed coupling with a C9–C15 fragment (7 or 8), may provide a common precursor of most palmerolides. Ligands and reaction conditions were exhaustively examined to perform the C15–C16 bond formation via Negishi reaction. With simple models, pre-activated Pd–Xantphos and Pd–DPEphos complexes were the most efficient catalysts at RT. Zincation of the C9–C15 fragment (8) and cross coupling with 4 required 3 equiv of t-BuLi, 10 mol % of Pd–Xantphos and 60 °C. 相似文献
18.
A series of neutral palladium(IV) hydride complexes supported by β-ketoimine ligands was synthesized. Reaction of dichlorobis(acetonitrile)palladium(II) with β-ketoamines (1–4) in dichloromethane at room temperature generated dark red solids of [PdCl2(β-ketoimine)(H)] (6–9) in which the central carbon of the ketoimine ligand is σ-bound to the palladium. All the new complexes have been characterized by NMR and IR spectroscopy. The structure of complex(9) has been solved by X-ray crystallography. 相似文献
19.
Xinru Liu Fuhang Song Li Ma Caixia Chen Xue Xiao Biao Ren Xueting Liu Huanqin Dai Andrew M. Piggott Yossef Av-Gay Lixin Zhang Robert J. Capon 《Tetrahedron letters》2013
Chemical analysis of an East China Sea marine-derived fungus, Aspergillus sydowii (MF357) returned three new tris-pyrogallol ethers, sydowiols A–C (1–3), and two known bis-pyrogallol ethers, violaceols I (4) and II (5). Structures were assigned on the basis of detailed spectroscopic analysis and by consideration of symmetry. Sydowiols A (1) and C (3) were responsible for the inhibitory activity detected in the crude fungal extract against Mycobacterium tuberculosis protein tyrosine phosphatase A (PtpA). 相似文献
20.
Noemí Andrade-López Tracy A. Hanna José G. Alvarado-Rodríguez Adriana Luqueño-Reyes Bernat A. Martínez-Ortega Daniel Mendoza-Espinosa 《Polyhedron》2010
Cis-diaquobis{di-(2-pyridyl)-N-ethylimine}nickel(II) chloride (2) was obtained from the reaction of di-(2-pyridyl)-N-ethylimine (1) and [NiCl2dppe] [dppe = cis-1,2-bis(diphenylphosphino)ethylene] in a 2:1 ratio in hot acetonitrile. Cis-dichloro{di-(2-pyridyl)-N-ethylimine}palladium(II) (3) and cis-dichloro{di-(2-pyridyl)-N-ethylimine}platinum(II) (4) complexes were obtained from the reaction of MCl2 (M = Pd, Pt) and (1) in equimolar ratio in hot acetonitrile. Compounds 1–4 were characterized by IR spectroscopy, elemental analysis, and mass spectrometry; the complexes 3 and 4 were characterized in solution by NMR. In addition, solid state structures of compounds 1–4 were determined using single crystal X-ray diffraction analyses. X-ray diffraction data of the complexes 3 and 4 showed a distorted square planar local geometry at palladium and platinum atoms with the chlorine atoms in a cis-coordination; in 2 a local octahedral geometry at nickel atom was observed. Complexes 3 and 4 are arranged as dimers with a M?M distance of 3.4567(4) Å (M = Pd) and 3.4221(4) Å (M = Pt), respectively; 2 consists of units linked by intermolecular hydrogen bonding. 相似文献