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1.
Summary. 2-Hydroxy-2,2-diphenylacetohydrazide (2), cyclic ketones, and mercaptoalkanoic acids were converted into 2-hydroxy-N-(3-oxo-1-thia-4-azaspiro[4.4]non/[4.5]dec-4-yl)-2,2-diphenylacetamide derivatives (3, 4) in a one pot procedure. Compounds 3 and 4 were tested for in vitro antimycobacterial activity against M. tuberculosis H37Rv. The compounds were found to provide 0–86% inhibition of mycobacterial growth in the primary screen conducted at 6.25 μg/cm3. 相似文献
2.
Fafu Yang Cuiyu Huang Hongyu Guo Jianrong Lin Qi Peng 《Journal of inclusion phenomena and macrocyclic chemistry》2007,58(1-2):169-172
The novel thiacalix[4]-1,3-2,4-aza-biscrown 3 in 1,3-alternate conformation, was facilely prepared by “1 + 2” cyclocondensation of p-tert-butylthiacalix[4]arene tetrahydrazide derivative 2 with o-phthalaldehyde in yield of 78%. The liquid–liquid extraction experiment showed that compound 3 was excellent receptor for zwitterionic α-amino acids and soft cations Ag+ and Hg2+. The extraction percentage of methionine was as high as 78%. 相似文献
3.
N. T. Pokhodylo R. D. Savka V. S. Matiichuk N. D. Obushak 《Russian Journal of General Chemistry》2009,79(2):309-314
By cycloaddition of arylazides to acetylacetone are obtained derivatives of 1,2,3-triazole. In the reaction of 1-[5-methyl-1-(R-phenyl)-1H-1,2,3-triazol-4-yl] ethanones (IIa–IIe) and 1-[4-(4-R-5-methyl-1H-1,2,3-triazol-1-yl)phenyl] ethanones (VIIa-VIIe) with isatin are obtained 2-[1-(R-phenyl)-5-methyl-1H-1,2,3-triazol-4-yl]-4-quinolinecarboxylic acids (IIIa–IIIe) and 2-[4-(4-R-5-methyl-1H-1,2,3-triazol-1-yl)phenyl] -4-quinolinecarboxylic acids (IXa, IXb), respectively. We found that 1-[5-methyl-1-(R-phenyl)-1H-1,2,3-triazol-4-yl] ethanones (IIa–IIe) readily transform into [5-methyl-1-(R-phenyl)-1H-1,2,3-triazol-4-yl] acetic acids (IVa–IVc) by the method of Wilgerodt-Kindler. The (5-methyl-1-phenyl-1H-1,2,3-triazol-4-yl)acetic acid reacts with 5-phenyl-4-amino-4H-1,2,4-triazol-3-thiol affording 6-[(5-methyl-1-phenyl-1H-1,2,3-triazol-4-yl) methyl]-3-phenyl[1,2,4] triazolo[3,4-b] [1,3,4] thiadiazole (VI).
Original Russian Text ? N.T. Pokhodylo, R.D. Savka, V.S. Matiichuk, N.D. Obushak, 2009, published in Zhurnal Obshchei Khimii,
2009, vol. 79, no. 2, pp. 320–325. 相似文献
4.
The preparation of 3-amino- and 3-dialkylamino-4-cyanoazepino[3,4-fc]indoles bearing substituents on the aromatic nucleus and N10 is outlined. Starting from suitable substituted ethyl 3-formylindole-2-carboxy-latcs 2 , condensation with malononitrile ( 3 ) and subsequent sodium borohydride-reduction yielded ethyl 3-(2,2-dicyanoethyl)indole-2-carboxylates 5 and 19 , respectively, which were cyclized in boiling alkoxides to 3-alkoxy-4-cyanoazepino[3,4-b]indoles 10,11,20 and 21 . This sequence constitutes a novel and flexible route to functional azepino[3,4-b>]indoles. The aminolysis of 10,11,20 and 21 with different amines and ammonia yielded the title compounds which were screened for their possible biological activity. 相似文献
5.
Wei Li Yun-Li Liu Jian Liu Huai-teng Zhang Shu-Zhong Zhan De-Rong Cao 《Transition Metal Chemistry》2011,36(3):255-260
The triazenide, 1-[(2-carboxyethyl)benzene]-3-[2-pyridine]triazene (HL), has been synthesized. In the presence of Et3N, the reaction of HL with Cu(OAc)2·H2O or CuCl2·2H2O gives the tetranuclear copper(II) complexes {Cu4(L)2(μ2-OH)2(OAc)4} 1 and {Cu4L4(μ4-O)Cl2} 2, respectively. The X-ray crystal structures of both complexes have been obtained. Magnetic studies indicate significant antiferromagnetic
coupling between the copper(II) centers for both complexes, with coupling constants (J) of −493.4 cm−1 for 1 and −165 cm−1 for 2. 相似文献
6.
V. Rajeswar Rao M. Madan Mohan Reddy 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):461-471
3-acetyl coumarins on condensation with various aromatic aldehydes in the presence of piperidine gave corresponding chalcones in a solid state under solvent free conditions. These chalcones are isolated and characterized. The in-situ-formed chalcones (1) are also converted into corresponding 2-aryl-4-[2H-2-oxo[1]benzopyran-3-yl]-2,3-dihydro (3) and 2,5-dihydro-1,5-benzothiazepines (4) in one step by interacting with orthoamino thiophenol. Both the 2,3-dihydro (3) and 2,5-dihydrobenzothiazepines (4) have been converted into same tetrahydrobenzothiazepine (5). Finally, the tetrahydrobenzo thiazepine (5) is converted into its acetyl derivative (11). The structures of the title compounds have been confirmed on the basis of their microanalytical, IR, 1 H NMR, and mass spectral data. 相似文献
7.
A. Shahrisa M. Zirak A. R. Mehdipour R. Miri 《Chemistry of Heterocyclic Compounds》2011,46(11):1354-1363
New symmetrical 4-[2-chloro-2-(4-chloro-6-methyl-2-oxo-2H-pyran-3-yl)vinyl]-substituted 1,4-di-hydropyridines were synthesized
in moderate to good yields via the modified Hantzsch reaction of β-dicarbonyl compounds with (Z)-3-chloro-3-(4-chloro-6-methyl-2-oxo-2H-pyran-3-yl)acrolein in the presence of an excess amount of NH4OAc. Also, the reaction of β-dicarbonyl compounds with (Z)-3-chloro-3-(4-chloro-6-methyl-2-oxo-2H-pyran-3-yl)acrolein in the presence of enamino esters and ketones was performed,
and asymmetrical 4-[2-chloro-2-(4-chloro-6-methyl-2-oxo-2H-pyran-3-yl)vinyl]-substituted 1,4-dihydropyridines were obtained
in moderate to good yields at room temperature. The calcium channel blocking activity of these compounds was assessed. They
demonstrated moderate to weak effects, although one compound had a comparable effect (IC50 =1.40×10−7 M) with respect to the reference drug Nifedipine. 相似文献
8.
超声辐射下合成1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲 总被引:2,自引:0,他引:2
1-苯基-3-甲基-5-氯吡唑-4-甲酸与氨基硫脲在三氯氧磷中反应得到2-氨基-5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑(1), 然后分别采用超声辐射法和常规加热法与(未)取代苯甲酰基异硫氰酸酯(2)反应合成了一系列未见报到的1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲(3a~3j). 化合物的结构经元素分析, IR, 1H NMR确证. 相似文献
9.
A. M. Magerramov R. A. Alieva V. I. Mardanova F. M. Chyragov A. V. Kurbanov K. A. Potekhin 《Journal of Structural Chemistry》2012,53(1):202-205
Single crystal X-ray diffraction is used to determine the crystal and molecular structure of 4-trifluoro-2-[2-(4-fluorophenyl)hydrazine-1-ylidene]-1-(thiophen-2-yl)butane-1,3-dione.
Crystallographic data for C14H8F4N2O2S are as follows: a = 8.2723(6) ?, b = 9.3009(7) ?, c = 9.9895(7) ?; α = 79.224(2)°, β = 75.851(2)°, γ = 72.337(2)°. Triclinic crystal system, P-1 space group, d
x = 1.622 g/cm3, V = 704.83(9) ?3, μ = 0.286 mm−1, crystal size 0.30×0.20×0.20 mm, R1 = 0.0891, wR2 = 0.1989. 相似文献
10.
Vikunjana K. Akbari Piyush P. Savaliya 《Phosphorus, sulfur, and silicon and the related elements》2013,188(5):711-719
Abstract A new series of 2-substituted-3-((3-(6-nitrobenzo[d]thiazol-2-yl)-4-oxo-3,4-dihydroquinazolin-2-yl)methyl)-1,3,4-thiadiazol-3-ium-5-thiolate 6(a–j) was synthesized starting from anthranilic acid 1. The structures of the newly synthesized compounds were characterized by IR, 1H NMR, 13C NMR, mass spectra, and elemental analysis. The final compounds were tested for their antimicrobial activity against several microbes. [Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental files: Additional text and tables.] 相似文献
11.
Hai-Bin Tian Duan-Zhi Yin Lan Zhang Li-Hua Wang Chun-Fu Zhang Jun-Ling Li Wei Zhou Chun-Ying Wu Yong-Xian Wang 《Journal of Radioanalytical and Nuclear Chemistry》2004,262(2):383-389
The compound 3-{[4-(4-[18F]fluorophenyl)methyl]piperazin-1-yl}-methyl-1H-pyrrolo[2,3-b]pyridine ([18F]3), which is an analogue of L-745,870 binding D4
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
12.
Peter Gajdoš Soňa Pavlíková Filip Bureš Alžbeta Krutošíková 《Central European Journal of Chemistry》2005,3(2):311-325
The synthesis and reactions of methyl 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole-5-carboxylate (1a) are described. Upon reaction with methyl iodide, benzyl chloride, or acetic anhydride, this compound gave N-substituted products 1b-d. By hydrolysis of compounds 1a-c, the corresponding acids 2a-c were formed, or by reaction with hydrazine-hydrate, the corresponding carbohydrazides 3a-c were formed. By heating 2-[3-(trifluoromethyl)phenly]-4H-furo[3,2-b]pyrrole-5-carboxylic acid (2a) in acetic anhydride, 4-acetyl-2-[3-(trifluoromethyl)phenyl]furo[3,2-b]pyrrole (4) was formed. By hydrolysis of 4, 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole (5a) was formed, and reactions with methyl iodide or benzyl chloride gave N-substituted products 5b-c. The reaction of 4 with dimethyl butynedioate gave substituted benzo[b]furan 6. Compound 3a reacted with triethyl orthoesters giving 7a-c, which afforded with phosphorus (V) sulphide the corresponding thiones 8a-c. The thiones 8a-c reacted with hydrazine hydrate to form hydrazine derivatives 9a-c. The reaction of triethyl orthoformiate with compounds 9a-c led to furo[2′,3′: 4,5]pyrrolo[1,2-d][1,2,4]triazolo[3,4-f][1,2,4]triazines 10a-c. Hydrazones 11a-c were formed from 3a-c and 5-[3-(trifluoromethyl)phenyl]furan-2-carboxaldehyde. The effect of microwave irradiation on some condensation reactions
was compared with “classical” conditions. The results showed that microwave irradiation shortens the reaction time while affording
comparable yields. 相似文献
13.
The crystals of 2-(6-chloro-4-(p-tolylamino)pyrido[3,2-d]pyrimidin-1-ium-1-yl)acetate (zwitterionic form) oxonium bromide, C16H13ClN4O2·Br−·H3O+ (I) were prepared and studied by single-crystal X-ray diffraction method. The compound crystallizes in the triclinic space group
P-1 with a = 8.3121(8) ?, b = 9.3885(8) ?, c = 13.2903(12)?, α = 106.788(2)°, β = 95.204(3)°, γ = 110.871(2)°, V = 905.81(14) ?3, Z = 2; final R = 0.053, wR2 = 0.150. It is interesting that methylene C in the BrCH2COOH molecule binds to the N1 of the pyrimidine ring. In the crystal studied, two neighboring organic molecules are connected
by hydrogen bonds through carboxylate oxygen, oxonium and bromide ions to form a dimer. 相似文献
14.
I. V. Konovalova V. F. Mironov G. A. Ivkova E. R. Zagidullina A. T. Gubaidullin I. A. Litvinov M. A. Kurykin 《Russian Journal of General Chemistry》2005,75(4):549-560
2-R-benzo[e][1,3,2]dioxaphosphinin-4-ones react with perfluorodiacetyl under mild conditions to form relatively labile spirophosphoranes containing a 1,3,2-dioxaphosphole ring. These compounds gradually convert to more stable 2-R-4,5-bis(trifluoromethyl)-1,3,2λ5-dioxaphosphole 2-oxides and diastereometic 2-R-4-(trifluoroacetyl)-4-(trifluoromethyl)benzo[f][1,3,2λ5]dioxaphosphepine 2-oxides, whose structure was confirmed by means of NMR and IR spectroscopy. The structure of 4′,5′ -bis(trifluoromethyl)-4-oxo-2-(2,2,3,3-tetrafluoropropoxy)-2λ 5-spiro[benzo[e][1,3,2]dioxaphosphinine-2,2′-[1,3,2]dioxaphosphole] was confirmed by X-ray diffraction analysis.__________Translated from Zhurnal Obshchei Khimii, Vol. 75, No. 4, 2005, pp. 587–599.Original Russian Text Copyright © 2005 by Konovalova, Mironov, Ivkova, Zagidullina, Gubaidullin, Litvinov, Kurykin. 相似文献
15.
N. K. Artemova V. A. Smirnov B. G. Rogachev G. V. Shilov S. M. Aldoshin 《Russian Chemical Bulletin》2006,55(9):1605-1611
1′,3′,3′-Trimethyl-6-nitro-8-pyridiniomethylspiro[2H-[1]benzopyran-2,2′-indoline] chloride (1) was synthesized. Single crystals (crystal hydrates) of the open merocyanine form of compound 1 were obtained under the dark conditions, and their crystal structure was studied. On irradiation with visible light compound
1 crystallizes from propan-2-ol in the polycrystalline closed form. The spectral and photochemical properties of compound 1 in the polycrystalline state and the kinetic characteristics on thermal transformation of the closed form to the open form
were studied.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1548–1553, September, 2006. 相似文献
16.
Ketalization of benzophenones with epichlorohydrin or 3-chloropropane-1,2-diol gave 2,2-diaryl-4-chloromethyl-1,3-dioxolanes,
which were used to alkylate sodium salts of imid-azole or 1,2,4-triazole. The resulting 1-[(2,2-diaryl-1,3-dioxolan-4-yl)methyl]-1H-azoles exhibit high fungicidal activities.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 940–944, May, 2007. 相似文献
17.
I. A. Mochalov A. N. Lapshin V. A. Nadtochenko V. A. Smirnov N. F. Goldshleger 《Russian Chemical Bulletin》2006,55(9):1598-1604
Axial coordination of fullerenopyrrolidine bearing the donor imidazolyl group, cis-3-(4-imidazolylphenyl)-1-(pyridin-2-yl)[60]fullereno[1,2-c]pyrrolidine (C60∼Im), with zinc meso-tetraphenylporphyrinate (ZnTPP) in an o-dichlorobenzene solution affords a non-covalently bonded donor-acceptor dyad ZnTPP-C60∼Im. The photochemical behavior of the ZnTPP-C60∼Im complex was studied by fluorescence (excitation at λ = 420 nm) and laser kinetic spectroscopy (excitation at λ = 532 nm,
12 ns). The formation constant of the 1: 1 porphyrin-fullerenopyrrolidine complex determined from quenching of ZnTPP fluorescence
assuming static intracomplex quenching is 1.6·104 L mol−1. Absorption spectra of the excited states in the system consisting of ZnTPP and Im∼C60 (ZnTPP/C60∼Im) were measured in solution from 380 to 1000 nm. The quenching constant of the triplet-excited ZnTPP with fullerenopyrrolidine
C60∼Im was determined. The results obtained indicate the formation of the triplet exciplex {PL}* ⇌ {Pδ+…Lδ−} in the ZnTPP/C60∼Im system upon laser photolysis.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1541–1547, September, 2006. 相似文献
18.
Two copper(I) complexes [Cu(Cin2bda)2]ClO4 (I) and [Cu(Ncin2bda)2]ClO4 (II) have been prepared by the reaction of the ligands N2,N2′-bis(3-phenylallylidene)biphenyl-2,2′-diamine (L1) and N2,N2′-bis[3-(2-nitrophenyl)allylidene]biphenyl-2,2′-diamine (L2) and copper(I) salt. These compounds were characterized by CHN analyses, 1H NMR, IR, and UV-Vis spectroscopy. The C=N stretching frequency in the copper(I) complexes shows a shift to a lower frequency
relative to the free ligand due to the coordination of the nitrogen atoms. The crystal and molecular structure of II was determined
by X-ray single-crystal crystallography. The coordination polyhedron about the copper(I) center in the complex is best described
as a distorted tetrahedron. A quasireversible redox behavior was observed for complexes I and II.
The article is published in the original. 相似文献
19.
Summary. A series of 1,5-disubstituted 3-(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl)-2-pyrazolines were synthesized by the reaction of α,β-unsaturated ketones derived from dehydroacetic acid and
hydrazine in hot acetic acid or propionic acid. The structures of all new compounds were elucidated by microanalyses, 1H and 13C NMR, IR, and mass spectroscopic measurements. 相似文献
20.
Bei Yan Guang-ji Wang Jian-guo Sun Fen-zhi Sun Xiao-yu Li Xiao-ming Wu Jin-yi Xu Yuan-ting Zheng Hua Lv 《Chromatographia》2007,66(1-2):55-61
A simple and sensitive reversed-phase LC-ESI-MS method to identify and quantitate 5-n-butyl-4-{4-[2-(1H-tetrazole-5-yl)-1H-pyrrol-1-yl]phenylmethyl}-2,4-dihydro-2-(2,6-dichloridephenyl)-3H-1,2,4-triazol-3-one (1b), a new Angiotensin II type 1 receptor antagonist in rat plasma has been developed and validated.
Sample preparation used a simple liquid–liquid extraction with ethyl acetate. Separation was achieved by gradient elution
on a C18 column. The mobile phase consisted of acetonitrile and water (0.05% triethylamine and 0.05% acetic acid) at a flow rate of
0.2 mL min−1. The detection utilized selected ion monitoring (SIM) in the negative mode at m/z 507.1 and m/z 407.2 for the deprotonated molecular ions of 1b and the internal standard irbesartan, respectively. The lower limit of quantification
was reproducible at 5 ng mL−1 with 100 μL of plasma and the good linear was observed in the 5–500 ng mL−1 range. This concentration range corresponded well with the plasma concentrations of 1b in pharmacokinetic studies. Recoveries
of 1b in rat plasma were 76.1, 74.6 and 79.0% at 5, 50 and 500 ng mL−1. The RSD of intra-assay and inter-assay variations were all less than 5%. This validated LC-ESI-MS assay is an economic,
quick, precise and reliable method for the analysis of 1b in pharmacokinetic studies. 相似文献