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1.
Issa Yavari Zinatossadat Hossaini Maryam Sabbaghan Majid Ghazanfarpour-Darjani 《Tetrahedron》2007,63(38):9423-9428
The reaction of ethyl propiolate with triphenylphosphine (Ph3P) in the presence of N-alkylisatins led to ethyl 2,2,2-triphenyl-2,5-dihydro-1,2-λ5-oxaphosphole-4-carboxylate-spiro-1-alkyl-1,3-dihydro-2H-indol-2-ones in good yield. The reaction of dialkyl acetylenedicarboxylates with Ph3P in the presence of N-alkylisatins led to dialkyl 2,2,2-triphenyl-2,5-dihydro-1,2-λ5-oxaphosphole-3,4-dicarboxylate-spiro-1-alkyl-1,3-dihydro-2H-indol-2-ones and alkyl 4-(alkoxy)-5-oxo-2,5-dihydro-3-furancarboxylate-spiro-1-alkyl-1,3-dihydro-2H-indol-2-ones. 相似文献
2.
L. G. Shagun I. A. Dorofeev I. A. Tokareva L. I. Larina M. G. Voronkov 《Russian Journal of Organic Chemistry》2012,48(12):1561-1563
Solvent-free reactions of 1,2,3-benzotriazole with 1-iodopropan-2-one and 1,3-diiodopropan-2-one in the absence of a catalyst involved alkylation of the heteroring at the N1 atom and subsequent quaternization at the N3 atom with formation of 1,3-bis(2-oxopropyl)-1H-1,2,3-benzotriazolium triiodide which is a new conducting ionic liquid. The reaction of 1,2,3-benzotriazole with 1,3-diiodopropan-2-one was accompanied by reductive deiodination of the iodomethyl groups in the initial ketone with hydrogen iodide liberated by N1-alkylation. Triiodide ion readily exchanges for nitrate ion by the action of AgNO3 to produce 1,3-bis(2-oxopropyl)-1H-1,2,3-benzotriazolium nitrate. The reaction of 1,2,3-benzotriazole with 2-iodo-1-phenylethan-1-one in melt resulted in the formation of 1,3-bis(2-oxo-2-phenylethyl)-1H-1,2,3-benzotriazolium triiodide. 相似文献
3.
Hetero-Diels–Alder reactions of perfluoroalkyl thioamides with electron-rich 1,3-dienes such as 2,3-dimethylbutadiene, isoprene or penta-1,3-diene gave a simple and efficient access to new 2-aminosubstituted-3,6-dihydro-2H-thiopyrans. Three different procedures were used depending on the nature of the polyfluoroalkyl chains (RF=CF3, (CF2)nCF3, (CF2)4H) and on the nitrogen substituents of the thioamides (R1, R2=H, p-Tol, morpholino, Ac). Moreover, cycloadditions of silyloxydienes (1- or 2-trimethylsilyloxy-1,3-butadiene and Danishefsky's diene) with N-acyl,N-tolyl trifluoromethylthioamides afforded in almost all cases the corresponding 3,6-dihydro-2H-thiopyrans or 3-oxo-tetrahydrothiopyrans. For non-symmetrical 1,3-dienes, the regio- and stereochemistry of the reactions were studied (especially using X-ray diffraction analysis) indicating a strong similarity with those reported for fluorinated thiocarboxyl derivatives. Finally, two silylated 3,6-dihydro-2H-thiopyrans underwent an unexpected base-induced ring contraction to give new 1,3-thiazolidin-4-ones. 相似文献
4.
A. A. Panasenko A. F. Kaprosh M. A. Rekhter E. P. Styngach M. Z. Krimer G. N. Grushetskaya 《Russian Chemical Bulletin》1994,43(3):391-394
13C NMR spectra (20 and 75 MHz, in DMSO-d6) of a series of 1,3-diaryl-3-(1H-1,2,4-triazol-1-yl)- and 1,3-diaryl-2-(1H-1,2,4-triazol-1-yl)prop-2-en-1-ones were registered. It was shown that the chemical shifts of both the carbon atom of the alkene group and C(3) reflect regio- and stereoisomerism of these compounds. Taking this into account the isomeric structures of several 1,3-diaryl-3-(1H-1,2,4-triazol-1-yl)prop-2-en-1-ones were identified and the configurations relative to the double bond of a number of 1,3-diaryl-2-(1H-1,2,4-triazol-1-yl)prop-2-en-1-ones were determined. 相似文献
5.
《Journal of organometallic chemistry》1989,364(3):C17-C21
3-Organo-1,3-benzazaphospholes and -benzazarsoles as well as 3,3-disubstituted 1,3-benzazasiloles and -benzazastannoles are prepared from o-LiC6H6NC(Li)But and the relevant organoelement dichlorides. The heterocycles obtained are converted by flash vacuum pyrolysis into the aromatic 1H-1,3-benzazaphospholes and benzazarsoles, respectively. 相似文献
6.
By reaction of [Ir(COD)Cl]2 (COD = 1,5-cyclooctadiene) with i-C3H7MgBr in the presence of cyclic dienes, complexes of the type [IrH(COD)L] (L = 1,3-cyclohexadiene, 2-methyl-],3-cyclohexadiene, 5-ethyl-1,3-cyclohexadiene, 1,3-cycloheptadiene) are obtained. The system IrCl3/i-C3H7MgBr/1,3-C6H8 yields [IrH(1,3-C6H8)2]. According to NMR spectroscopic investigations the pure hydrido forms exist in solution only at low temperatures while at room temperature dynamic H-addition—elimination equilibria of the type [IrH(η4-diene)(COD)] ? [Ir(η3-enyl)(COD)] and [IrH(η4-1,3-C6H8)2] ? [Ir(η3-C6H9)-(η4-1,3-C6H8)], respectively, are observed; the hydrogen at the iridium atom is thereby transferred to the endo positions of the diene ligands. 相似文献
7.
The reactions of RCo(BDM1,3pn)(H2O) with light, heat, acids, electrophiles and nucleophiles were studied. (HBDM1,3pn is a mononegative, tetradentate dioxime-diimine ligand formed by condensing 2,3-butanedionemonoxime with 1,3-propanediamine in a 2/1 molar ratio; R = CH3, C2H5, n-C3H7, n-C4H9, and C6H3CH2-) Pyrolysis and photolysis of the alkyl complexes result in a cobalt(II) complex (anaerobic conditions) along with alkenes and alkanes. The major organic products from solid state pyrolysis at 200°C or photolysis in water are CH4 (R = CH3), C2H4 (R = C2H5), C3H6 (R = n-C3H7), C4H8 (R = n-C4H9) and (C6H5CH2)2 (R = C6H5CH2). No alkyl—cobalt bond cleavage occurs with acids or bases in most cases. Two exceptions are the reactions with 3 M HNO3 at 25°C and with 1 M NaOH at 52°C. Electrophiles like I2 cleave the alkyl—cobalt bond forming RI and CoIII (BDM1,3pn)I2. Nucleophilic reagents (N-) displace the H2O trans to the alkyl group to form RCo(BDM1,3pn)(N), but do not dealkylate the alkyl complex under the reaction conditions studied. 相似文献
8.
A series of hetero-dinuclear CuII-ZnII complexes, [CuZnCl2L1] (1), [CuZnCl2L2] (2), [CuZnBr2L3] (3), [CuZnBr2L4(DMF)] (4), [CuZnCl2L4] (5), [CuZnCl2L5] (6), [CuZnCl2L3] (7) and [CuZnBr2L1] (8), where L1, L2, L3, L4 and L5 are the deprotonated forms of N,N′-bis(3-ethoxysalicylidene)-1,3-propanediamine (H2L1), N,N′-bis(2-hydroxynaphthylmethylidene)-1,3-propanediamine (H2L2), N,N′-bis(3-methoxysalicylidene)-1,3-propanediamine (H2L3), N,N′-bis(salicylidene)-1,3-propanediamine (H2L4) and N,N′-bis(salicylidene)-1,4-butanediamine (H2L5), respectively, have been synthesized and characterized by physico-chemical methods and single-crystal X-ray diffraction. The complexes were tested for their urease inhibitory activity. Complexes 1 and 8 show effective urease inhibitory activity with IC50 values of 2.2 and 10.7 μM. The molecular docking study of the complexes with the Helicobacter pylori urease was performed. 相似文献
9.
《Journal of Saudi Chemical Society》2014,18(3):190-199
In the present study two new series of Copper(II), Nickel(II) and Cobalt(II) complexes with two newly synthesized Schiff base ligands 4,6-bis(1-(4-bromophenylimino)ethyl)benzene-1,3-diol (H2L1), 4,6-bis(1-(4-methoxyphenylimino) ethyl)benzene-1,3-diol (H2L2) and organic ligands 8-hydroxy quinoline, 1,10-phenanthroline have been prepared. The Schiff bases H2L1 and H2L2 ligands were synthesized by the condensation of 4,6-diacetyl resorcinol with 4-bromo aniline and 4-methoxy aniline. The ligands and their metal complexes have been characterized by FT-IR, Mass, 1H NMR, UV–Vis., elemental analysis, ESR and Thermal gravimetric analysis. The Schiff base and their metal complexes were tested for antimicrobial activity against gram positive bacteria Staphylococcus aureus, Streptococcus pyogenes and gram negative bacteria Escherichia coli, Pseudomonas aeruginosa and fungus Candida albicans, Aspergillus niger and Aspergillus clavatus using Broth Dilution Method. 相似文献
10.
S. V. Safronov A. M. Sheloumov P. V. Petrovskii M. G. Ezernitskaya A. A. Koridze 《Russian Chemical Bulletin》2012,61(11):2065-2069
The reaction of [CpRu(CH3CN)3][PF6], [Cp*RuCl] n , and [CpFRuCl]n with 1,3-diformylindene results in the predominant formation of zwitter-ionic arene-cyclopentadienyl complexes {η6-1,3-(CHO)2C9H5}RuCp (Cp = C5H5), {η6-1,3-(CHO)2C9H5}RuCp* (Cp* = C5Me5), and {η6-1,3-(CHO)2C9H5}RuCpF (CpF = C5Me4CF3), respectively. The ruthenocenes {η5-1,3-(CHO)2C9H5}RuCp, {η5-1,3-(CHO)2C9H5}RuCp*, and {η5-1,3-(CHO)2C9H5}RuCpF were synthesized by the reaction of 1,3-diformylindenyl potassium with [CpRu(CH3CN)3][PF6], [Cp*RuCl] n , and [CpFRuCl] n . 相似文献
11.
Preliminary reactions of the metal stabilized carbocationic species [(η-C5H5)Ni(μ-η2(Ni),η3(Mo)-HC2CMe2)Mo(CO)2(η-C5H4Me)]+ BF4− (Ni-Mo) with nucleophiles are reported. The Ni-Mo cationic propargylic complex undergoes nucleophilic attack by sodium methoxide to regenerate the neutral μ-alkyne complex [(η-C5H5)Ni{μ-η2,η2-HC2CMe2(OMe)}Mo(CO)2(η-C5H4Me)] (Ni-Mo), from which the stabilized carbocation was originally derived by protonation. The new complexes [(η-C5H5)Ni{μ-η2,η2-HC2CMe2(C5H5)}Mo(CO)2(η-C5H4Me)] (Ni-Mo), which exist as an inseparable mixture of 1(c)-1,3- and 2(c)-1,3-cyclopentadienyl isomers, were also obtained. When the Ni-Mo cations were treated with potassium t-butoxide, the alkyne isomers with pendant 1(c)-1,3- and 2(c)-1,3-cyclopentadienyl groups are also formed. The μ-hydroxyalkyne complex [(η-C5H5)Ni{μ-η2,η2-HC2CMe2(OH)}-Mo(CO)(η-C5H4Me)] (Ni-Mo) was also isolated concurrently, and presumably arises from nucleophilic attack of fortuitously present hydroxide ions in the BuO− reagent on the Ni-Mo cation. When NaBH4 was added to the Ni-Mo propargylic, nucleophilic attack by hydride resulted and the μ-iPrC2H heterobimetallic complex [(η-C5H5)Ni{μ-η2,η2-HC2Pri}Mo(CO)2(η-C5H4Me)] (Ni-Mo) was recovered in good yield. Small quantities of other side-products were isolated and characterized spectroscopically. Some tantalizing differences in reactivity were observed when the corresponding Ni-W stabilized carbocation was reacted with methoxide ions. When the not fully characterized solid formed by protonating [(η-C5H5)Ni(μ-η2,η2-{HC2CMe2)(OMe)}W(CO)2(η-C5H4Me)] (Ni-W) was treated with methoxide ions, regioisomers (1(c)-1,3- and 2(c)-1,3-cyclopentadienyl species) of composition [(η-C5H5)Ni{μ-η2,η2-HC2CMe2(C5H5)}W(CO)2(η-C5H4Me)] (Ni-W) were formed. Direct reaction of the pure cation [(η-C5H5Niμ-η2,η3-HC2CMe2)W(CO)2(η-C5H4Me)]+ (Ni-W) with methoxide also generated the same 1(c)-1,3- and 2(c)-1,3-cyclopentadiene-substituted alkyne complexes. Unlike the case with the Ni-Mo complexes, the initial μ-HC2CMe2(OMe) species was not regenerated. 相似文献
12.
You-Gui Huang 《Journal of solid state chemistry》2009,182(2):215-9497
Three lanthanide-organic frameworks formulated as [Yb2(1,3-pda)3(H2O)]n·nH2O (1) [La2(2,5-pydc)3(H2O)2]n (2) and [La(2,5-pydc)(2,5-Hpydc)(H2O)2]n·nH2O (3) (H21,3-pda=1,3-phenylenediacetic acid, H22,5-pydc=pyridine-2,5-dicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. Both the frameworks of compounds 1 and 2 exhibit intricate 3D architectures which can be simplified as nets with mixed nodes. Compound 1 presents a very complicated net with five types of nodes comprising intersecting (3,4)-connected and CdSO4 nets. Compound 2 possesses a (4,4,6)-connected net with (4284)(4462)2(4966)2 circuit symbol. While compound 3 is a 2D layer based upon carboxyl-bridged LaIII chains. 相似文献
13.
Unique thiocyanate-connected 1-dimensional chain Cu(II) coordination polymer (CP), namely, [Cu2L1(μ1,3-SCN) (η1SCN)]n (1), was produced in the existence of KSCN and Cu(NO3)2·3H2O utilizing an underlying multisite N,O donor Schiff base ligand (L1H2). [N,N′-bis(3-methoxysalicylidenimino)-1,3-daminopropane] (L1H2), the Schiff base ligand is a 1:2 M ratio condensation product of 1,3-diaminopropane and O-vaniline in the methanol medium. The as-created CP 1 has been investigated with various characterization approaches like powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), -thermogravimetric analysis (TGA) and single crystal X-ray diffraction (SCXRD) analyses. And the mechanism and therapeutic effect of this CP on sepsis was discussed and its specific mechanism was also assessed. First of all, for the infected animals, their survival rate was recorded after the bacterial infection and treatment of complex. Besides this, utilizing the enzyme linked immunosorbent assay (ELISA) assay, the inflammatory cytokines levels that released into plasma were determined after the exposure of compound. 相似文献
14.
A series of seven novel f-element bearing hybrid materials have been prepared from either methyl substituted 3,4 and 4,5-pyrazoledicarboxylic acids, or heterocyclic 1,3- diketonate ligands using hydrothermal conditions. Compounds 1, [UO2(C6H4N2O4)2(H2O)], and 3, [Th(C6H4N2O4)4(H2O)5]·H2O feature 1-Methyl-1H-pyrazole-3,4-dicarboxylate ligands (SVI-COOH 3,4), whereas 2, [UO2(C6H4N2O4)2(H2O)], and 4, [Th(C6H5N2O4)(OH)(H2O)6]2·2(C6H5N2O4)·3H2O feature 1-Methyl-1H-pyrazole-4,5-dicarboxylate moieties (SVI-COOH 4,5). Compounds 5, [UO2(C13H15N4O2)2(H2O)]·2H2O and 6, [UO2(C11H11N4O2)2(H2O)]·4.5H2O feature 1,3-bis(4-N1-methyl-pyrazolyl)propane-1,3-dione and 1,3-bis(4-N1,3-dimethyl-pyrazolyl)propane-1,3-dione respectively, whereas the heterometallic 7, [UO2(C11H11N4O2)2(CuCl2)(H2O)]·2H2O is formed by using 6 as a metalloligand starting material. Single crystal X-ray diffraction indicates that all coordination to either [UO2]2+ or Th(IV) metal centers is through O-donation as anticipated. Room temperature, solid-state luminescence studies indicate characteristic uranyl emissive behavior for 1 and 2, whereas those for 5 and 6 are weak and poorly resolved. 相似文献
15.
Condensation of Betti base analogue amino naphthols with substituted benzaldehydes led to 1,3-diaryl-2,3-dihydro-1H-naphth[1,2-e][1,3]oxazines (3-9) which proved to be three-component (r1-o-r2) tautomeric mixtures in CDCl3 at 300 K. The electronic effects of the 3-aryl groups on the ratios of the ring-chain tautomeric forms at equilibrium could be described by the equation log KX=ρσ++log KX=H. The value of the intercept was found to be strongly influenced by the steric arrangement of the 1,3-diaryl substituents. 相似文献
16.
T. S. Zyubina L. V. Shmygleva R. V. Pisarev A. S. Zyubin A. V. Pisareva Yu. A. Dobrovolsky 《Russian Chemical Bulletin》2012,61(8):1521-1530
Hydrate clusters of 2-hydroxybenzenesulfonic and 1,3-benzenedisulfonic acids were calculated in terms of the density functional theory (DFT) by the B3LYP/6-31G** method. The process of water adsorption on the crystal surface of 4-hydroxy-1,3-benzenedisulfonic acid dihydrate was simulated using the generalized gradient approximation (DFT/PBE) and periodic boundary conditions. For the model system (OHC6H4SO3 ?)·H5O2 +, the activation barriers for the proton transfer were calculated depending on the distance between the O atoms and the deviation of the proton from the O...O bond line. The presence of one H2O molecule per SO3H group is energetically most favorable for the formation of clusters of 1,3-benzenedisulfonic acid containing a stoichiometric amount of water. The simulation of the hydration of 4-hydroxy-1,3-benzenedisulfonic acid dihydrate (OHC6H3(SO3H)2·2 H2O + n H2O, n = 1–3) showed that the superstoichiometric H2O molecule is adsorbed on the crystal surface of this dihydrate with energy release of 0.75–0.95 eV. The position of this water molecule is less favorable in the bulk than on the surface. 相似文献
17.
Mohammad El-khateeb Mousa Al-Noaimi Noor Al-Rejjal Hassan Abul Fetouh Helmar Görls Wolfgang Weigand 《Transition Metal Chemistry》2013,38(5):529-534
A series of thiocarboxylato and selenocarboxylato monomeric CpFe(CO)2ECORCOCl and dimeric [CpFe(CO)2ECO]2R iron complexes have been synthesized and characterized. The interaction of (μ-Ex)[CpFe(CO)2]2 (E = S; x = 2–4. E = Se; x = 1) with di-acid chlorides (ClCORCOCl) in a 1:1 molar ratio gave the monomeric complexes CpFe(CO)2ECORCOCl for R = 1,3-C6H4, 2,6-C5H3N, 1,2-C6H4. However, the dimeric complexes [CpFe(CO)2ECO]2R were obtained from the same reactants in a 2:1 metal-to-ligand molar ratio in which R is 1,3-C6H4, 2,6-C5H3N or C2H4. The monomer versus dimer production mainly depends on the electronic and steric factors of the R-moiety. The new monomeric and dimeric thio- and selenocarboxylato iron complexes have been characterized by spectroscopic techniques (1H- and 13C-NMR, IR) and by elemental analysis. The structures of [CpFe(CO)2SCO]2(1,3-C6H4) and its seleno analogue [CpFe(CO)2SeCO]2(1,3-C6H4) were determined by X-ray structure determination. 相似文献
18.
《Tetrahedron: Asymmetry》2001,12(10):1469-1474
Chiral dithioether ligands have been tested in the model Pd-catalysed allylic alkylation reaction of (±)-3-acetoxy-1,3-diphenyl-1-propene with dimethyl malonate, giving high enantioselectivity (up to 81% e.e.) for the first time in this type of system. Pd(II)-allylic intermediates, [Pd(η3-1,3-Ph2-C3H3)(dithioether)]PF6 were prepared and characterised both in solution by NMR spectroscopy and solid state. The X-ray structure for [Pd(η3-1,3-Ph2-C3H3)(L)]PF6 (L=(R,R)-7,8-O-isopropylidene-1,5-dithia-cyclononane) was determined. 相似文献
19.
1-Hydroxy-2-chloromethyl-1,3-dioxolane (4) and 1-hydroxy-2-dichloromethyl-1, 3-dioxolane (5) have been detected as intermediates by1H NMR spectroscopy in the hydration of respectively 2-chloromethylene-1, 3-dioxolane and 2-dichloromethylene-1, 3-dioxolane in aqueous acetonitrile. The kinetics of the breakdown of (4) and (5) into ethylene glycol monochloroacetate and monodichloroacetate have been studied by uv spectroscopy and values ofkH+,kHO-, andkH2O evaluated. It was found that the introduction of chlorosubstituents into 2-hydroxy-2-methyl-1, 3-dioxolane caused a decrease inkH+ and increase inkH2O- and little change inkH2Ofor its breakdown. The mechanisms of these reactions are discussed. Present 相似文献
20.
The dealkylation of a variety of RCo(BDMBg)+ complexes by Hg2+ is discussed. (The ligand BDMBg- is formed by the condensation of two moles of 2,3-butanedionemonoxime with one mole of 1,3-propanediamine or 1,2-ethanediamine.) The products of the dealkylation reaction are CoIII(BDMBg)(H2O)2+2 and RHg+. All reactions are first order in the [Hg2+]. The second order rate constants (k2) vary from 5.9 M-1 sec-1 (R = CH3) to 5.7 x 10-3M-1 sec-1 (R = n-C3H7). The relative rates for R are: CH3 ? C2H5 τ C6H5CH2 τ n-C4H9 ? n-C3H7. This order and other evidence are indicative of an SE2 mechanism with an attack by Hg2+ on the carbon bonded to the cobalt. 相似文献