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1.
Madarász J. Bombicz P. Jármi K. Bán M. Pokol G. Gál S. 《Journal of Thermal Analysis and Calorimetry》2002,69(1):281-290
Thermal stability and structural features of three newly synthesized 1:1 lattice compounds of theophylline (th) with ethylenediamine carbamate (enCO2), 1,10-phenanthroline (phen), and 5-sulfosalicylic acid (sa-5-SO3H) have been studied in comparison with those of the theophylline compounds with ethanolamine (ea) and salicylic acid (sa). Simultaneous TG-DTA measurements, FTIR spectroscopy and X-ray diffraction have been carried out to get information on the various structural units of these solid inclusions, especially on the actual form (molecule, anion or cation) of theophylline moieties built in. Theophyllinate and theophyllinium ions have been found in the ethanolammonium-theophyllinate (1:1) (1, eaH+th-) and the theophyllinium salicylic acid 5-sulfonate monohydrate (1:1:1), (5, thH+saSO–3H2O), respectively. Whilst the 1:1 complexes with 1,10-phenanthroline (2, thphen), ethylenediamine carbamate (3, thenCO2), and salicylic acid (4, thsa) contain neutral theophylline moieties associated with H-bonds. In compound (3) the zwitterion of N-(2-ammonium-ethyl)carbamate (NH3+-CH2-CH2-NH-CO-2) is present.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
2.
Yan-Qiu Yang Cheng-Fu Su Jun-Di Zhang Gui-Yang Zhang 《Journal of Coordination Chemistry》2016,69(24):3762-3775
Three new Cd(II) complexes incorporating both 2-(1H-imidazol-1-methyl)-1H-benzimidazole (imb) and 1,4-benzenedicarboxylate (bdic2?), [CdCl(bdic)1/2(imb)2]n (1), {[Cd(bdic)(imb)(H2O)]·DMF·2H2O}n (2), and [Cd(bdic)(imb)]·3H2O}n (3), have been prepared and structurally characterized by single crystal X-ray diffraction. Bdic2? anions connect the?Cd-imb-Cd-imb?chains leading to a 2-D structure of 1. Bdic2?(A) and bdic2?(B) anions link the binuclear [Cd2(imb)2(H2O)2] units forming a 2-D structure of 2. Complex 3 features a 2-D structure involving supramolecular “double-layer” motifs. IR spectra and thermogravimetric curves are consistent with the results of the X-ray crystal structure analysis; 1–3 exhibit good fluorescence in the solid state at room temperature. 相似文献
3.
The reactions of 5,5-dimethyl-3-oxo-1-pyrroline 1-oxide (3-oxo-DMPO, 1) with NH2OH and N2H4 afforded oxime (2a) and hydrazone (2b), respectively. The reaction products were studied as spin traps for the short-lived radicals HO·, Ph·, PhCO2
·, NC(Me2)C·, and NC(Me2)CO·. The nitroxides generated in the reactions of the above-mentioned short-lived radicals with nitrones 1 and 2a,b were characterized by ESR spectroscopy. Of these nitrones, oxime 2a is the most effective radical trap. 相似文献
4.
E. V. Tretyakov S. V. Fokin G. V. Romanenko V. N. Ikorskii A. V. Podoplelov V. I. Ovcharenko 《Russian Chemical Bulletin》2006,55(1):66-73
An efficient procedure was developed for the synthesis of alkyltetrazolyl-substituted nitronyl nitroxides (L
1 and L
2). These compounds were used to prepare the first alkyltetrazolyl-substituted imino nitroxides (L
3 and L
4). The molecular structures of L
3 and L
4 were confirmed by X-ray diffraction. Investigation of the products prepared by the reaction of copper(II) bis(hexafluoroacetylacetonate), Cu(hfac)2, with nitroxides made it possible to divide ligands L
1—L
4 into two groups. The reactions of spin-labeled tetrazoles L
1—L
3 with Cu(hfac)2 afford the heterospin complexes Cu(hfac)2L2, whereas L
4 serves as a bidentate ligand in the Cu(hfac)2
L
4 complex. In the solid Cu(hfac)2L2 complexes, antiferromagnetic exchange interactions between the unpaired electrons of the nitroxide fragments of the adjacent
molecules prevail, due to which μeff decreases with decreasing temperature, and the spins of nitroxides are completely compensated at 5–10 K. The Cu(hfac)2
L
4 complex displays strong intramolecular ferromagnetic coupling, due to which μeff at room temperature is close to 2.9 μB.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 64–70, January, 2006. 相似文献
5.
6.
Liu Meng De-Qing Shi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):2314-2323
A series of title compounds 2 were efficiently synthesized via the condensation of 1-phenyl-2-(1H-1,2,4-triazol-1-yl)ethanone oxime with various asymmetric thiophosphoryl chlorides in sodium hydroxide powder and acetonitrile system. The structures of title compounds 2 were confirmed by IR, 1H NMR, 31P NMR, EI-MS, and elemental analysis. The results of preliminary bioassays indicated that the title compounds 2 possessed good to moderate insecticidal activity against aphides at the dosage of 250 mg/L, and some of them exhibited moderate fungicidal activities at the concentration of 100 mg/L. 相似文献
7.
Oscar P. Rodriguez Thomas M. Lane Sheldon E. Cremer 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4)
Abstract During our investigations on the wide range of stereoselective alkylations of 6-membered ring phostones,1 we uncovered a novel rearrangement of 3-(diphenylhydroxymethyl)-2-ethoxy-2-oxo-1,2-oxaphosphorinane (1). The cis/trans diastereomers of 1 were prepared by the reaction of benzophenone with the appropriate ylide of the parent phostone (3).2 When trans- 1 was left unattended at rt in CH2Cl2 a new compound, 2, was isolated which showed a significant downfield 31P shift and a higher melting point. Upon heating to the melting point 2 decomposed to give 4, which suggests that 2 may be an intermediate in the conversion of 1 to the Wittig-like product 4. The IR, 1H, 13C, 31P, and 2-D NMR spectral data along with independent synthesis confirmed the identity of 2. Subsequently, 2 was also produced in 70% yield when cis- 1 was treated with CH2Cl2/ether-HC1aq at 50–60°C for 2 weeks, but this product was contaminated with 30% of the exocyclic alkene 5. No rearrangement was observed when 1 was treated with TsOH/EtOH or HPF6; only 5 was produced. The stereochemistry and mechanisms of these transformations are presented. 相似文献
8.
《Journal of Coordination Chemistry》2012,65(7):1224-1237
Two new cobalt(II) complexes, [Co(L3)2]·CH3OH·CH3COCH3 (1) (HL3 = 1-(2-{[(E)-3,5-dichloro-2-hydroxybenzylidene]amino}phenyl)ethanone oxime) and Co(L4)2 (2) (HL4 = 1-(2-{[(E)-3,5-dibromo-2-hydroxybenzylidene]amino}phenyl)ethanone oxime), have been synthesized via complexation of Co(II) acetate tetrahydrate with HL1 and HL2. HL1, HL2, and their corresponding Co(II) complexes were characterized by IR, 1H NMR spectra, as well as by elemental analysis and UV–Vis spectroscopy, respectively. The crystal structures of the complexes have been determined by single-crystal X-ray diffraction. 1 and 2 display that extensive hydrogen bonds and C–X···π bonding interactions construct the 1-D infinite chain [Co(L3)2]·CH3OH·CH3COCH3 and Co(L4)2 into 2-D supramolecular frameworks. The electrochemical properties of two Co(II) complexes were also investigated by cyclic voltammetry. 相似文献
9.
10.
《Journal of Coordination Chemistry》2012,65(9):1584-1595
Three coordination polymers of Robson-type macrocycles, {[Cu4L1(4,4′-bipy)2]·4ClO4·H2O}∞ (1), {[Cu4L2(4,4′-bipy)4]·2CH3CN·4ClO4·2H2O}∞ (2), and {[Zn2L2(4,4′-bipy)2]·(ClO4)2}∞ (3) (where H2L1 and H2L2 are the [2?+?2] condensation products of 1,3-diaminopropane with 2,6-diformyl-4-methylphenol and 2,6-diformyl-4-fluorophenol, respectively), have been synthesized and characterized. Magnetic susceptibility was measured for 1 and 2 from 2 to 300?K. The optimized magnetic data were J?=?–368.5?cm?1, J′?=?40.5?cm?1 with R?=?1.69?×?10?6 for 1 and J?=?–291.22?cm?1, J′?=?83.74?cm?1, ρ = 0.00168 with R?=?1.8?×?10?11 for 2, respectively. The data reveal strong antiferromagnetic interactions between two Cu(II) ions in the macrocyclic unit and ferromagnetic interaction between the Cu(II) ions in two adjacent macrocyclic units for 1 and 2. 相似文献
11.
Ambika Chopra Pooja Sharma 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):208-219
12.
Vasile-Nicolae Bercean Valentin Badea Călin Deleanu Alina Nicolescu 《Central European Journal of Chemistry》2012,10(2):373-379
1H-1-Alkyl-6-methyl-3-phenyl-7-phenylazopyrazolo[5,1-c][1,2,4]triazoles (2aa-ad) were obtained by regioselective alkylation of 1H-6-methyl-3-phenyl-7-phenylazopyrazolo[5,1-c][1,2,4]triazoles (2a). 1H-1-Alkyl-6-methyl-3-phenyl-7-phenylazopyrazolo[5,1-c][1,2,4]triazoles 2aa and 2ab were also prepared by coupling phenyldiazonium chloride with 1H-1-alkyl-6-methyl-3-phenyl-pyrazolo[5,1-c][1,2,4]triazoles 1aa and 1ab. The new compounds were characterized by IR, UV-VIS, 1H-NMR, 13C-NMR, and 15N-NMR spectroscopy and their structures and actual tautomeric forms were established unequivocally.
相似文献
13.
1-Phenylamino-2-imidazoline und 1,2,5,6-Tetrahydro-1,2,4-triazine aus N-(2-Chloralkyl)-imidchloriden
Jörg Beger Renate Neumann Dieter Scheller 《Monatshefte für Chemie / Chemical Monthly》1981,112(8-9):959-971
1-Phenylamino-2-imidazolines3 and 1,2,5,6-tetrahydro-1,2,4-triazines4, 5 and6 are synthesized from N-(2-chloralkyl)-imidchlorides1 and phenylhydrazines. As intermediates are obtained the hydrochlorides of amidrazones2 which cyclise. The structure of the different heterocyclic systems are determined by1H- and13C-NMR-spectroscopy. 相似文献
14.
Alex F. C. Flores Mauro J. Martins Leandro M. Frigo Pablo Machado Patrick T. Campos Juliana L. Malavolta 《合成通讯》2013,43(5):727-737
Novel 1-aryl-4,4,4-trichloro-1,3-butanediones in good yields (80–97%) were synthesized in one pot through acetal acylation with trichloroacetyl chloride followed by acid hydrolysis. Structures of all compounds were elucidated by elemental analysis, mass spectrometry, and 1H/13C nuclear magnetic resonance (NMR) measurements. The 1H/13C NMR data showed that trichloromethyl-β-diketones 2a–k in solution are predominantly ketoenol. However, the spectroscopic data from 4,4,4-trichloro-2-methyl-1-phenyl-1,3-butabedione (2l) with methyl substituent between carbonyls showed a bias toward the diketo form in solution. X-ray diffraction of monocrystals from 2g and 2i showed that these compounds are cis-ketoenol tautomers. Supplemental materials are available for this article. Go to the publisher's online edition of Synthetic Communcations® to view the free supplemental file. 相似文献
15.
M. N. Bochkarev T. V. Balashova A. A. Maleev I. I. Pestova G. K. Fukin E. V. Baranov Yu. A. Kurskii 《Russian Chemical Bulletin》2008,57(10):2162-2167
The reactions of phthalonitrile with MeNH2, PrnNH2, and PriNH2 in the presence of catalytic amounts of LnI3 (Ln = Nd or Dy) or LnI3(THF)3 (Ln = Gd or Nd) afford 1,3-bis(alkylimino)isoindolines (Alk = Me (1), Prn (2), or Pri (3), respectively). Under analogous conditions, 2-aminopyridine gives 1,3-bis(2-pyridylimino)isoindoline (4). The X-ray diffraction study of compound 3 showed that, in the crystalline state, this compound exists as the isomer, 1-isopropylamino-3-(isopropylimino)isoindole. 相似文献
16.
K. N. Shavrin I. V. Krylova I. E. Dolgii O. M. Nefedov 《Russian Chemical Bulletin》1992,41(5):885-891
1,1-Dichloro-2-alkynes R1CCCHCl2 (4a–g; R1=Me, n-Pr, c-Pr, t-Bu, Ad, Nor, Ph) were synthesized with yields of 50–75% by chlorination with PCl5 of formylacetylenes (3a–g), prepared by oxidation of propargyl alcohols (1a–d) with CrO3·Py·HCl complex or acidolysis of propargyl acetals (2a–c) in the presence of catalytic quantities of pyridine; the corresponding alkynylchlorocarbenes, R1CCCCl (5a–g) were generated from them with powdered KOH in a two-phase system or t-BuOK. The latter were trapped by olefins with formation of 1-chloro-1-alkynylcyclopropanes (6a–t) with yields of up to 90%.See [1] for Communication 1.N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, 117913 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 5, pp. 1128–1135, May, 1992. 相似文献
17.
18.
J. Halász G. Tóth I. Kádas G. Árvai K. Mikló R. Haeßner 《Monatshefte für Chemie / Chemical Monthly》1995,126(8-9):1011-1019
Summary Base catalyzedMichael addition of 5-nitropentan-2-one ethylene ketal (1) and cyclohex-2-enone (2), subsequent deprotection, and intramolecular aldol condensation yields the 8-methyl-5-nitro-1-octalone isomers (5a,b). The structure, relative configuration, and conformation of5a and5b were elucidated utilizing the results of1H and13C NMR investigations
Synthese und Stereochemie von 8-Methyl-5-nitro-octalonen
Zusammenfassung BasenkatalysierteMichael-Addition von 5-Nitropentan-2-on-ethylenketal (1) und Cyclohex-2-enon (2), anschließende Entfernung der Schutzgruppe und darauffolgende Aldolkondensation liefert isomer 8-Methyl-5-nitro-1-octalone (5a,b). Struktur, relative Konfiguration und Konformation von5a und5b wurden mittels1H- und13C-NMR-Spektroskopie aufgeklärt.相似文献
19.
Nikolay Kaloyanov Mihail Neykov Diana W. Wesselinova Georgi D. Dimitrov 《Central European Journal of Chemistry》2012,10(4):1034-1041
Novel heavy metal complexes: Sr(5-NH2-phen)4(NO3)(OH)(H2O)2 (1) (synthesized via a static self-assembly process) and Sn(phen)(NO3)(OH)(H2O) (2), Sn(5-NH2-phen)(OH)(Cl)(H2O) (3), Pb(5-NH2-phen)(NO3)2(H2O) (4) (obtained via metal competitive reactions under mild conditions) were reported. The coordination compounds were characterized by elemental
analysis, FTIR-spectroscopy and FAB-mass spectrometry. Their cytotoxicity was measured by MTS-test towards human tumour (MDA-MB-231,
HT-29, HeLa, HepG2) and non-tumour diploid (Lep-3) cell lines. The most pronounced cytotoxic effect on all cancer lines showed
1 and 4 at their high concentrations as well as 1 at its lower ones (≤ 4×10−2 mg). Therefore, strontium complex of 5-amino-o-phenanthroline (1) exhibited the widest antitumour spectrum activity, having no toxicity to non-tumour cells at quantities ≤ 4×10−2 mg. The computed EC50 values of 1–4 against MDA-MB-231, HT-29, HeLa, HepG2 varied from 1.40×10−3 to 6.31×10−6 M. Towards Lep-3 substances 2–4 showed IC50 7.52×10−4 − 0.44 M. Substance 1 possess EC50=1.26×10−7 M to the non-tumour cells.
相似文献
20.
N. A. Shtel’tser S. V. Osintseva P. V. Petrovskii A. Z. Kreindlin F. M. Dolgushin 《Russian Chemical Bulletin》2006,55(12):2143-2148
The reaction of Ru3(CO)12 with 2-methyl-3-morpholino-1-phenylprop-2-en-1-one (1) produced the Ru6(CO)16(μ4-η1:η1:η2:η2-PhC(O)-C(Me)=C)2 (2), Ru2O2(CO)4(η3-OC(Ph)C(Me)C(H)C(Me)2C(Ph))2 (3), and [Ru(CO)2(PhCO2)(O(CH2-CH2)2NH]2 (4) complexes, which were characterized by IR and NMR spectroscopy. The structures of the complexes were established by X-ray
diffraction. The formation of the complexes is accompanied by deamination of ligand 1. Complexes 2 and 3 bearing the vinyl ketone groups contain five-membered oxaruthenacycles and dihydropyran rings. Morpholine is not removed
from the reaction mixture and leads to the formation of complex 4.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2063–2068, December, 2006. 相似文献