First-principles calculations of a high-pressure synthesized compound PtC

International Nuclear Information System (INIS)

Li Linyan; Yu Wen; Jin Changqing

2005-01-01

The first-principles density-functional method is used to study the recently high-pressure synthesized compound PtC. It is confirmed by our calculations that platinum carbide has a zinc-blende ground-state phase at zero pressure and that the rock-salt structure is a high-pressure phase. The theoretical transition pressure from zinc-blende to rock-salt structure is determined to be 52 GPa. Furthermore, our calculation shows the possibility that the PtC experimentally synthesized under high pressure conditions might undergo a transition from rock-salt to zinc-blende structure after a pressure quench to ambient conditions

Luminescence properties of Tb{sub 3}Al{sub 5}O{sub 12} garnet and related compounds synthesized by the metal organic decomposition method

Energy Technology Data Exchange (ETDEWEB)

Onishi, Yuya; Nakamura, Toshihiro, E-mail: tnakamura@gunma-u.ac.jp; Adachi, Sadao, E-mail: adachi@gunma-u.ac.jp

2017-03-15

The Tb–Al–O ternay compounds were prepared by the metal organic decompostion (MOD) method from mixted solutions of Al{sub 2}O{sub 3} and Tb{sub 4}O{sub 7} and subsequent calcination at T{sub c}=1200 °C in air. The structural and optical properties of the synthesized compounds were examined using X-ray diffraction analysis, photoluminescence (PL) analysis, PL excitation (PLE) spectroscopy, PL decay kinetics, and diffuse reflectance spetrosopy. The stoichiometric compounds of terbium aluminium garnet Tb{sub 3}Al{sub 5}O{sub 12} (TAG) and peroviskite-type TbAlO{sub 3} were synthesized at molar ratios of x=0.375 and 0.5 [x ≡Tb{sub 4}O{sub 7}/(Tb{sub 4}O{sub 7}+2Al{sub 2}O{sub 3})], together with the end-point binary materials of rhombohedral Al{sub 2}O{sub 3} (α-Al{sub 2}O{sub 3}; x=0) and cubic Tb{sub 4}O{sub 7} (x=1.0). One can also expect synthesis of stoichiometric compounds Tb{sub 4}Al{sub 2}O{sub 9} and Tb{sub 3}AlO{sub 12} at x=0.667 and 0.75, respectively; however, these compounds were found to be very difficult to synthesize by the MOD method or, probably by other methods. Temperature dependence of the PL spectra for TAG was measured from T=20–440 K in 10-K step and analyzed using a newly developed theoretical model. Raman scattering measurements were also performed on the Tb–Al–O material system with compositions widely varying from x=0 (α-Al{sub 2}O{sub 3}) to 1.0 (Tb{sub 4}O{sub 7}).

Design, Synthesis and Biological Evaluation of 1,4-Disubstituted-3,4-dihydroisoquinoline Compounds as New Tubulin Polymerization Inhibitors

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Ling Zhang

2015-05-01

Full Text Available A series of 1,4-disubstituted-3,4-dihydroisoquinoline derivatives designed as tubulin polymerization inhibitors were synthesized. Their cytotoxic activities against the CEM leukemia cell line were evaluated. Most of them displayed moderate cytotoxic activities, and compounds 21 and 32 showed good activities with IC50 of 4.10 and 0.64 μM, respectively. The most potent compound 32 was further confirmed to be able to inhibit tubulin polymerization, and its hypothetical binding mode with tubulin was obtained by molecular docking.

Hydrogen bonded supra-molecular framework in inorganic-organic hybrid compounds: Syntheses, structures, and photoluminescent properties

Science.gov (United States)

Yan, Li; Liu, Wei; Li, Chuanbi; Wang, Yifei; Ma, Li; Dong, Qinqin

2013-03-01

Two novel compounds constructed from aromatic acid and N-Heterocyclic ligands have been synthesized by hydrothermal reaction: [Cd(mip)(1,8-NDC)(H2O)]2 (1) [mip = 2-(3-methoxyphenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, 1,8-NDC = naphthalene-1,8-dicarboxylic acid] and Cd(mip)2(NTC)2 (2) [NTC = nicotinic acid]. Compounds 1 and 2 are characterized by elemental analysis, IR, single crystal X-ray diffraction and thermogravimetric analysis (TGA). Single-crystal X-ray investigation reveals that compounds 1-2 are 0 dimensional (0D) structures, and the existence of hydrogen bonds and π-π interactions lead the 0D to 2D novel framework. Hydrogen bonds and π-π interactions are powerful non-covalent intermolecular interactions for directing supra-molecular architectures. TG analysis shows clear courses of weight loss, which corresponds to the decomposition of different ligands. At room temperature, compound 1 exhibits emission at 449 nm upon excitation at 325 nm, and compound 2 shows a strong emission at 656 nm upon excitation at 350 nm. Fluorescent spectrum displays that compounds 1 and 2 are potential luminescent materials.

Construction of New Coordination Polymers from 4’-(2,4-disulfophenyl)- 3,2’:6’3”-terpyridine: Polymorphism, pH-dependent syntheses, structures, and properties

Energy Technology Data Exchange (ETDEWEB)

Zhang, Li; Li, Chao-Jie; He, Jia-En; Chen, Yin-Yu [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Zheng, Sheng-Run, E-mail: zhengsr@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, Guangzhou, 510006 (China); Fan, Jun [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Zhang, Wei-Guang, E-mail: wgzhang@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, Guangzhou, 510006 (China)

2016-01-15

Nine new coordination compounds, namely, [Co(HDSPTP){sub 2}(H{sub 2}O){sub 4}]·4H{sub 2}O (H{sub 2}DSPTP=4’-(2,4-disulfophenyl)-3,2’:6’3”-terpyridine, 1 and 2), {[Ni(DSPTP)(H_2O)_4]·3H_2O}{sub n} (3), {[Cu(HDSPTP)_2(H_2O)_3]·8H_2O}{sub n} (4), {[Cu(HDSPTP)_2(H_2O)_3]·6H_2O}{sub n} (5), {[Cu(DSPTP)(H_2O)_2]·H_2O}{sub n} (6), {[Zn(DSPTP)(H_2O)_2]·2H_2O}{sub n} (7), {[Cd(DSPTP)(H_2O)_2]·2H_2O}{sub n} (8), and [Ag{sub 2}(DSPTP)(H{sub 2}O)]{sub n} (9), were constructed based on a new ligand containing both terpyridyl and sulfo groups. The reactions of H{sub 2}DSPTP with Co(NO{sub 3}){sub 2}.6H{sub 2}O resulted in two mononuclear complexes (compounds 1 and 2). They are polymorphisms that display different hydrogen bonding networks. They are selectively synthesized by altering the added alkalis. The reaction of H{sub 2}DSPTP with Ni(NO{sub 3}){sub 2}·6H{sub 2}O resulted in a 1D “S-shaped” coordination chain (compound 3). The reactions of Cu(II) with H{sub 2}DSPTP at different pH value resulted in the following three compounds: two kinds of 1D chains obtained at pH 3.0 and 4.0 for compounds 4 and 5, respectively, and a 3D framework based on binuclear ring units with 4-connected sra topology (Compound 6). The reactions of H{sub 2}DSPTP with ds-block ions resulted in the following three compounds: a Zn(II) (compound 7) and a Cd(II) (compound 8) 3D frameworks with structures similar to that in compound 6, and a 3D framework based on tetranuclear Ag(I) SBUs with binodal (4,8)-connected flu type 3D framework topology. The structural diversity is mainly attributed to the rich coordination modes (from monodentate to µ{sub 7}-mode) and conformations (cis–cis and cis–trans) of HDSPTP{sup −}/DSPTP{sup 2−} ligands and the metal center and can be controllable synthesized by altering the alkalis, and pH value. Thermal stability of all compounds was performed, and the thermal behaviors of compounds 6 and 8 were further explored by PXRD. Compound 6 exhibits

In vitro cytotoxicity and apoptotic inducing activity of the synthesized 4-aryl-4H-chromenes derivatives against human cancer cell lines

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Mohagheghi MA

2009-09-01

Full Text Available "n Normal 0 false false false EN-US X-NONE AR-SA MicrosoftInternetExplorer4 /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-qformat:yes; mso-style-parent:""; mso-padding-alt:0in 5.4pt 0in 5.4pt; mso-para-margin:0in; mso-para-margin-bottom:.0001pt; mso-pagination:widow-orphan; font-size:11.0pt; font-family:"Calibri","sans-serif"; mso-ascii-font-family:Calibri; mso-ascii-theme-font:minor-latin; mso-fareast-font-family:"Times New Roman"; mso-fareast-theme-font:minor-fareast; mso-hansi-font-family:Calibri; mso-hansi-theme-font:minor-latin; mso-bidi-font-family:Arial; mso-bidi-theme-font:minor-bidi;} Background: 4-Aryl-4H-chromenes are novel anticancer agents which induce apoptosis in cancer cells. These compounds were found to induce apoptosis by targeting the tubulin/microtubule system in cell proliferation process. The aim of this study was to report cyototoxic and apoptosis inducing activities of a new series of synthesized 4-aryl-4H-chromenes compounds."n"n Methods: The in vitro cytotoxic activity of the synthesized 4-aryl-4H-chromenes was investigated against a paned of human cancer cell lines including MCF-7 (breast carcinoma, A549 (lung carcinoma, HEPG-2 (liver carcinoma, SW-480 (colon adenocarcinoma, U87-MG (glioblastoma, 1321N1 (astrocytoma, and DAOY (medulloblastoma. The percentage of growth inhibitory activity was evaluated using MTT colorimetric assay versus controls not treated with test derivatives. The data for etoposide, a well known anticancer drug, was included for comparison. For each compound, the 50% inhibitory concentration (IC50 were determined. Apoptosis inducing activity were assessed by DAPI staining."n"n Results: Preliminary screening showed that those chromenes analogs bearing phenyl-isoxazole-3-yl substitution or the derivatives containing methoxyphenyl in chromene ring exhibited

Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids

KAUST Repository

Groh, Matthias Friedrich

2013-01-01

The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, α-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14),Bi8(AlCl4)2, Bi6Cl7,and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low-temperature syntheses in room temperature ionic liquids (RTILs). The simple one-pot syntheses generally do not require elaborate equipment such as twozone furnaces or evacuated silica ampoules. Compared to the published conventional approaches, reduction of reaction time (up to 80%) and temperature (up to 500 K) and, simultaneously, an increase in yield were achieved. In the majority of cases, the solid products were phase-pure. X-Ray diffraction on single crystals (redetermination of 11 crystal structures) has demonstrated that the quality of the crystals from RTILs is comparable to that of products obtained by chemical transport reactions. © 2013 Verlag der Zeitschrift für Naturforschung, Tübingen.

Synthesis and Antioxidant Activity Evaluation of New Compounds from Hydrazinecarbothioamide and 1,2,4-Triazole Class Containing Diarylsulfone and 2,4-Difluorophenyl Moieties

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Stefania-Felicia Barbuceanu

2014-06-01

Full Text Available In the present investigation, new hydrazinecarbothioamides 4–6 were synthesized by reaction of 4-(4-X-phenylsulfonylbenzoic acids hydrazides (X= H, Cl, Br 1–3 with 2,4-difluorophenyl isothiocyanate and further these were treated with sodium hydroxide to obtain 1,2,4-triazole-3-thione derivatives 7–9. The reaction of 7–9 with α-halogenated ketones, in basic media, afforded new S-alkylated derivatives 10–15. The structures of the synthesized compounds have been established on the basis of 1H-NMR, 13C-NMR, IR, mass spectral studies and elemental analysis. The antioxidant activity of all compounds has been screened. Hydrazinecarbothioamides 4–6 showed excellent antioxidant activity and 1,2,4-triazole-3-thiones 7–9 showed good antioxidant activity using the DPPH method.

Synthesis of Novel Heterocyclic Compounds Incorporate 4,5,6,7-Tetrahydrobenzo[b]thiophene Together with Their Cytotoxic Evaluations.

Science.gov (United States)

Abdallah, Amira Elsayed Mahmoud; Mohareb, Rafat Milad; Khalil, Eid Metwally; Elshamy, Menna Alla Mohamed Abd Elaleem

2017-01-01

The 2-amino-3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophene was the key starting compound used to synthesize new thiazole, pyrimidine, pyran, pyridine and thiazine derivatives. The cytotoxicity of the synthesized compounds was studied towards the three cancer cell lines namely MCF-7 (breast adenocarcinoma), NCI-H460 (non-small cell lung cancer) and SF-268 (central nervous system (CNS) cancer) in addition to the normal cell line (WI-38) using doxorubicin as the reference drug. The study showed that compounds 5, 9a, 15b, 17c, 18 and 21b were the most potent compounds.

ADP-ribosyl-N₃: A Versatile Precursor for Divergent Syntheses of ADP-ribosylated Compounds.

Science.gov (United States)

Li, Lingjun; Li, Qianqian; Ding, Shengqiang; Xin, Pengyang; Zhang, Yuqin; Huang, Shenlong; Zhang, Guisheng

2017-08-14

Adenosine diphosphate-ribose (ADP-ribose) and its derivatives play important roles in a series of complex physiological procedures. The design and synthesis of artificial ADP-ribosylated compounds is an efficient way to develop valuable chemical biology tools and discover new drug candidates. However, the synthesis of ADP-ribosylated compounds is currently difficult due to structural complexity, easily broken pyrophosphate bond and high hydrophilicity. In this paper, ADP-ribosyl-N₃ was designed and synthesized for the first time. With ADP-ribosyl-N₃ as the key precursor, a divergent post-modification strategy was developed to prepare structurally diverse ADP-ribosylated compounds including novel nucleotides and peptides bearing ADP-ribosyl moieties.

Combustion synthesized nanocrystalline Li3V2(PO4)3/C cathode for lithium-ion batteries

International Nuclear Information System (INIS)

Nathiya, K.; Bhuvaneswari, D.; Gangulibabu; Kalaiselvi, N.

2012-01-01

Graphical abstract: Nanocrystalline Li 3 V 2 (PO 4 ) 3 /C compound has been synthesized using a novel corn assisted combustion (CAC) method, wherein the composite prepared at 850 °C is found to exhibit superior physical and electrochemical properties than the one synthesized at 800 °C (Fig. 1). Despite the charge disproportionation of V 4+ and a possible solid solution behavior of Li 3 V 2 (PO 4 ) 3 cathode upon insertion and de-insertion of Li + ions, the structural stability of the same is appreciable, even with the extraction of third lithium at 4.6 V (Fig. 2). An appreciable specific capacity of 174 mAh g −1 with an excellent columbic efficiency (99%) and better capacity retention upon high rate applications have been exhibited by Li 3 V 2 (PO 4 ) 3 /C cathode, thus demonstrating the feasibility of CAC method in preparing the title compound to best suit with the needs of lithium battery applications. Display Omitted Highlights: ► Novel corn assisted combustion method has been used to synthesize Li 3 V 2 (PO 4 ) 3 /C. ► Corn is a cheap and eco benign combustible fuel to facilitate CAC synthesis. ► Li 3 V 2 (PO 4 ) 3 /C exhibits an appreciable specific capacity of 174 mAh g −1 (C/10 rate). ► Currently observed columbic efficiency of 99% is better than the reported behavior. ► Suitability of Li 3 V 2 (PO 4 ) 3 /C cathode up to 10C rate is demonstrated. -- Abstract: Nanocrystalline Li 3 V 2 (PO 4 ) 3 /C composite synthesized using a novel corn assisted combustion method at 850 °C exhibits superior physical and electrochemical properties than the one synthesized at 800 °C. Despite the charge disproportionation of V 4+ and a possible solid solution behavior of Li 3 V 2 (PO 4 ) 3 cathode upon insertion and extraction of Li + ions, the structural stability of the same is appreciable, even with the extraction of third lithium at 4.6 V. An appreciable specific capacity of 174 mAh g −1 and better capacity retention upon high rate applications have been

New effective chemically synthesized anti-smallpox compound NIOCH-14.

Science.gov (United States)

Mazurkov, Oleg Yu; Kabanov, Alexey S; Shishkina, Larisa N; Sergeev, Alexander A; Skarnovich, Maksim O; Bormotov, Nikolay I; Skarnovich, Maria A; Ovchinnikova, Alena S; Titova, Ksenya A; Galahova, Darya O; Bulychev, Leonid E; Sergeev, Artemiy A; Taranov, Oleg S; Selivanov, Boris A; Tikhonov, Alexey Ya; Zavjalov, Evgenii L; Agafonov, Alexander P; Sergeev, Alexander N

2016-05-01

Antiviral activity of the new chemically synthesized compound NIOCH-14 (a derivative of tricyclodicarboxylic acid) in comparison with ST-246 (the condensed derivative of pyrroledione) was observed in experiments in vitro and in vivo using orthopoxviruses including highly pathogenic ones. After oral administration of NIOCH-14 to outbred ICR mice infected intranasally with 100 % lethal dose of ectromelia virus, it was shown that 50 % effective doses of NIOCH-14 and ST-246 did not significantly differ. The 'therapeutic window' varied from 1 day before infection to 6 days post-infection (p.i.) to achieve 100-60 % survival rate. The administration of NIOCH-14 and ST-246 to mice resulted in a significant reduction of ectromelia virus titres in organs examined as compared with the control and also reduced pathological changes in the lungs 6 days p.i. Oral administration of NIOCH-14 and ST-246 to ICR mice and marmots challenged with monkeypox virus as compared with the control resulted in a significant reduction of virus production in the lungs and the proportion of infected mice 7 days p.i. as well as the absence of disease in marmots. Significantly lower proportions of infected mice and virus production levels in the lungs as compared with the control were demonstrated in experiments after oral administration of NIOCH-14 and ST-246 to ICR mice and immunodeficient SCID mice challenged with variola virus 3 and 4 days p.i., respectively. The results obtained suggest good prospects for further study of the chemical compound NIOCH-14 to create a new smallpox drug on its basis.

Hydrothermal chemistry of Th(IV) with aromatic dicarboxylates: New framework compounds and in situ ligand syntheses

International Nuclear Information System (INIS)

Ziegelgruber, Kate L.; Knope, Karah E.; Frisch, Mark; Cahill, Christopher L.

2008-01-01

A novel thorium (IV) coordination polymer, Th(C 5 H 2 N 2 O 4 ) 2 (H 2 O) 2 (1), has been prepared under the hydrothermal reaction of thorium nitrate tetrahydrate and 3,5-pyrazoledicarboxylic acid (H 3 pdc). Compound 1 (orthorhombic, P2 1 2 1 2 1 , a=6.9362(5) A, b=10.7806(8) A, c=17.9915(14) A, Z=2, R 1 =0.0210, wR 2 =0.0470) consists of thorium metal centers connected via H 3 pdc linkages to form an overall three-dimensional structure containing π-π interactions between the pyrazole rings. 2,3-Pyrazinedicarboxylic acid (H 2 pzdc) was explored as well to (1) study the effect of the location of the carboxylic groups around the aromatic ring and (2) produce heterometallic compounds. Thorium (IV) and copper (II) were combined with H 2 pzdc, resulting in an interesting decomposition reaction characterized though the isolation of Th(C 2 O 4 ) 2 (H 2 O) 2 .2H 2 O (2) (monoclinic, C2/c, a=13.8507(12) A, b=7.8719(7) A, c=10.7961(16) A, β=118.0310(10) o , Z=2, R 1 =0.0160, wR 2 =0.0349), Cu(C 6 H 2 N 2 O 4 ) (3) (monoclinic, C2/c, a=11.499(3) A, b=7.502(2) A, c=7.402(2) A, β=93.892(5) o , Z=4, R 1 =0.0472, wR 2 =0.0745) and Cu(C 5 H 3 N 2 O 2 )(NO 3 )(H 2 O) (4). The capture of these species provides mechanistic evidence for the formation of the oxalate anions observed in 2 via the decarboxylation of H 2 pzdc to yield the linker in 4: 2-pyrazinecarboxylate anions. - Graphical abstract: 3,5-Pyrazoledicarboxylic and 2,3-pyridinedicarboxylic acid were utilized in synthesizing two novel thorium (IV) coordination polymers. Attempts to synthesize a Th-Cu bimetallic compound with 2,3-pyridinedicarboxylic acid resulted in a triphasic mixture (2, 3 and 4, respectively). The oxalate anion observed in Th(C 2 O 4 ) 2 (H 2 O) 2 .2H 2 O (2) is theorized to result from decarboxylation of 2,3-pyridinedicarboxylic acid as supported by the organic linker, 2-pyrazinecarboxylate, observed in Cu(C 5 H 3 N 2 O 2 )(NO 3 )(H 2 O) (4)

Syntheses of Novel 4-Substituted N-(5-amino-1H-1,2,4-triazol-3-ylpyridine-3-sulfonamide Derivatives with Potential Antifungal Activity

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Krzysztof Szafrański

2017-11-01

Full Text Available Candidiasis represent a serious threat for patients with altered immune responses. Therefore, we have undertaken the synthesis of compounds comprising a pyridine-3-sulfonamide scaffold and known antifungally active 1,2,4-triazole substituents. Thus a series of novel 4-substituted N-(5-amino-1H-1,2,4-triazol-3-ylpyridine-3-sulfonamides have been synthesized by multistep reactions starting from 4-chloropyridine-3-sulfonamide via N′-cyano-N-[(4-substitutedpyridin-3-ylsulfonyl]carbamimidothioates which were further converted with hydrazine hydrate to the corresponding 1,2,4-triazole derivatives 26–36. The final compounds were evaluated for antifungal activity against strains of the genera Candida, Geotrichum, Rhodotorula, and Saccharomycess isolated from patients with mycosis. Many of them show greater efficacy than fluconazole, mostly towards Candida albicans and Rhodotorula mucilaginosa species, with MIC values ≤ 25 µg/mL. A docking study of the most active compounds 26, 34 and 35 was performed showing the potential mode of binding to Candida albicans lanosterol 14α-demethylase. Also in vitro cytotoxicity of selected compounds have been evaluated on the NCI-60 cell line panel.

Bifunctional properties of hydrothermal synthesized BaMF4 (M = Co, Ni and Zn

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Farheen N. Sayed

2013-07-01

Full Text Available BaMF4 (M = Co, Ni and Zn samples having orthorhombic structure have been synthesized by a mild hydrothermal method and characterized by x-ray diffraction (XRD, magnetic and electrical measurements. Single phase formation of these compounds has been found to be dependent on various factors like reaction time, pH, temperature etc. All the samples showed ferroelectricity, which decreases with increase in temperature. BaMF4 (M = Co, Ni samples show 10-15 times more leakage current compared to that of BaZnF4 at higher applied field. Absence of multivalent ions in BaZnF4 can be the reason for its minimum leakage current. All the samples except, BaZnF4, exhibit weak room temperature ferromagnetism also.

Facile Syntheses and Molecular-Docking of Novel Substituted 3,4-Dimethyl-1H-pyrrole-2-carboxamide/carbohydrazide Analogues with Antimicrobial and Antifungal Properties

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Jitendra D. Bhosale

2018-04-01

Full Text Available The article describes the use of facile one-pot, high-yielding reactions to synthesize substituted 3,4-dimethyl-1H-pyrrole-2-carboxamides 3a–m and carbohydrazide analogues 5a–l as potential antifungal and antimicrobial agents. The structural identity and purity of the synthesized compounds were assigned based on appropriate spectroscopic techniques. Synthesized compounds were assessed in vitro for antifungal and antibacterial activity. The compounds 5h, 5i and 5j were found to be the most potent against Aspergillus fumigatus, with MIC values of 0.039 mg/mL. The compound 5f bearing a 2, 6-dichloro group on the phenyl ring was found to be the most active broad spectrum antibacterial agent with a MIC value of 0.039 mg/mL. The mode of action of the most promising antifungal compounds (one representative from each series; 3j and 5h was established by their molecular docking with the active site of sterol 14α-demethylase. Molecular docking studies revealed a highly spontaneous binding ability of the tested compounds in the access channel away from catalytic heme iron of the enzyme, which suggested that the tested compounds inhibit this enzyme and would avoid heme iron-related deleterious side effects observed with many existing antifungal compounds.

Ferroelectric and magnetic properties in high-pressure synthesized BiFeO3 compound

International Nuclear Information System (INIS)

Zhai, L.; Shi, Y.G.; Gao, J.L.; Tang, S.L.; Du, Y.W.

2011-01-01

Highlights: → A high-density polycrystalline BiFeO 3 compound was synthesized by high-pressure annealing method. → The sample showed weak ferromagnetic at room temperature, which could be attributed to the lattice distortion induced by the high-pressure annealing. → Irregular domains were observed on the surface of the sample by piezoresponse force microscopy, and a typical hysteresis loop was obtained. - Abstract: High-density polycrystalline BiFeO 3 compound was synthesized by high-pressure annealing. Measurements of crystal structure, magnetic, and ferroelectric properties were made on the sample. It was found that the sample was almost single phase with a distorted R3c structure. The results of the X-ray photoelectron spectra demonstrate that the oxidation state of Fe in the sample is Fe 3+ . The room-temperature field dependence of magnetization for BiFeO 3 exhibits a hysteretic behavior. The observed weak ferromagnetism could be ascribed to the lattice distortion induced by the high-pressure annealing. In addition, the local ferroelectric performance of the sample was studied by piezoresponse force microscopy.

Synthesis and Anticancer Activity of New 1-Thia-4-azaspiro[4.5]decane, Their Derived Thiazolopyrimidine and 1,3,4-Thiadiazole Thioglycosides

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Eman M. Flefel

2017-01-01

Full Text Available New 1-thia-azaspiro[4.5]decane derivatives, their derived thiazolopyrimidine and 1,3,4-thiadiazole compounds were synthesized. The thioglycoside derivatives of the synthesized (1,3,4-thiadiazolylthiaazaspiro[4.5]decane and thiazolopyrimidinethione compounds were synthesized by glycosylation reactions using acetylated glycosyl bromides. The anticancer activity of synthesized compounds was studied against the cell culture of HepG-2 (human liver hepatocellular carcinoma, PC-3 (human prostate adenocarcinoma and HCT116 (human colorectal carcinoma cell lines and a number of compounds showed moderate to high inhibition activities.

Synthesis and antimicrobial activity of some novel fused heterocyclic 1,2,4-triazolo [3,4-b][1,3,4] thiadiazine derivatives

Science.gov (United States)

Sahu, Jagdish K.; Ganguly, Swastika; Kaushik, Atul

2014-01-01

In the present investigation, the synthesis and antimicrobial evaluation of 1,2,4-triazolo [3,4-b][1,3,4] thiadiazine including different pharmacophores are aimed at. In this study, a series of 6-aryl-3- (3,4 -dialkoxyphenyl)-7H -[1,2,4]triazolo [3,4-b][1,3,4] thiadiazine (7a-7k) was synthesized by condensing 4-amino-5-(3,4-dialkoxyphenyl)-4H-[1,2,4]- triazole-3-thiol (6) with various aromatic carboxylic acids in the presence of phenacyl bromides through one-pot reaction. Eleven fused heterocyclic derivatives were successfully synthesized. The structures of these newly synthesized compounds were characterized by IR, 1H NMR and mass spectroscopic studies. All the synthesized compounds were screened for their antimicrobial evaluation. Some of the compounds exhibited promising antimicrobial activity. From the present study it may be concluded that synthesized compounds are fruitful in terms of their structural novelty and marked biological activities. These compounds could be further modified to develop potential and safer antifungal agents. PMID:24959418

Syntheses and properties of several metastable and stable hydrides derived from intermetallic compounds under high hydrogen pressure

Energy Technology Data Exchange (ETDEWEB)

Filipek, S.M., E-mail: sfilipek@unipress.waw.pl [Institute of High Pressure Physics PAS, ul. Sokolowska 29, 01-142 Warsaw (Poland); Paul-Boncour, V. [ICMPE-CMTR, CNRS-UPEC, 2-8 rue Henri Dunant, 94320 Thiais (France); Liu, R.S. [Department of Chemistry, National Taiwan University, Taipei 106, Taiwan (China); Jacob, I. [Unit Nuclear Eng., Ben Gurion University of the Negev, Beer-Sheva (Israel); Tsutaoka, T. [Dept. of Sci. Educ., Grad. School of Educ., Hiroshima University, Hiroshima (Japan); Budziak, A. [Institute of Nuclear Physics PAS, 31-342 Kraków (Poland); Morawski, A. [Institute of High Pressure Physics PAS, ul. Sokolowska 29, 01-142 Warsaw (Poland); Sugiura, H. [Yokohama City University, 22-2 Seto, Kanazawa-ku, Yokohama 236-0027 (Japan); Zachariasz, P. [Institute of Electron Technology Cracow Division, ul. Zablocie 39, 30-701 Krakow (Poland); Dybko, K. [Institute of Physics, PAS, 02-668 Warsaw (Poland); Diduszko, R. [Tele and Radio Research Institute, ul. Ratuszowa 11, Warsaw (Poland)

2016-12-01

Brief summary of our former work on high hydrogen pressure syntheses of novel hydrides and studies of their properties is supplemented with new results. Syntheses and properties of a number of hydrides (unstable, metastable or stable in ambient conditions) derived under high hydrogen pressure from intermetallic compounds, like MeT{sub 2}, MeNi{sub 5}, Me{sub 7}T{sub 3}, Y{sub 6}Mn{sub 23} and YMn{sub 12} (where Me = zirconium, yttrium or rare earth; T = transition metal) are presented. Stabilization of ZrFe{sub 2}H{sub 4} due to surface phenomena was revealed. Unusual role of manganese in hydride forming processes is pointed out. Hydrogen induced phase transitions, suppression of magnetism, antiferromagnetic-ferromagnetic and metal-insulator or semimetal-metal transitions are described. Equations of state (EOS) of hydrides submitted to hydrostatic pressures up to 30 GPa are presented and discussed.

Synthesis and Antimicrobial Activity of New Schiff Base Compounds Containing 2-Hydroxy-4-pentadecylbenzaldehyde Moiety

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Gadada Naganagowda

2014-01-01

Full Text Available Various novel Schiff base compounds have been synthesized by reaction of 2-hydroxy-4-pentadecylbenzaldehyde with substituted benzothiophene-2-carboxylic acid hydrazide and different substituted aromatic or heterocyclic amines in the presence of acetic acid in ethanol. The structures of all these compounds were confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR, and mass spectral data and have been screened for antibacterial and antifungal activity.

Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids

KAUST Repository

Groh, Matthias Friedrich; Mü llera, Ulrike; Ahmed, Ejaz; Rothenberger, Alexander; Ruck, Michael J.

2013-01-01

The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, α-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14),Bi8(AlCl4)2, Bi6Cl7,and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low

Electric conduction mechanism of some heterocyclic compounds, 4,4′-bipyridine and indolizine derivatives in thin films

Energy Technology Data Exchange (ETDEWEB)

Danac, Ramona, E-mail: rdanac@uaic.ro [Faculty of Chemistry, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Leontie, Liviu, E-mail: lleontie@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Carlescu, Aurelian, E-mail: carlescu_aurelian@yahoo.com [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Shova, Sergiu, E-mail: shova@icmpp.ro [Petru Poni Institute of Macromolecular Chemistry, Aleea Grigore Ghica Voda, Nr. 41A, 700487 Iasi (Romania); Tiron, Vasile, E-mail: vasile.tiron@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Rusu, George G., E-mail: rusugxg@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Iacomi, Felicia, E-mail: iacomi@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Gurlui, Silviu, E-mail: sgurlui@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Șușu, Oana, E-mail: oasusu@gmail.com [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania); Rusu, Gheorghe I., E-mail: girusu@uaic.ro [Faculty of Physics, Alexandru Ioan Cuza University of Iasi, Bulevardul Carol I, Nr. 11, 700506 Iasi (Romania)

2016-08-01

Temperature dependence of d. c. electric conductivity of some recently synthesized heterocyclic compounds, 4,4′-bipyridine and indolizine derivatives, in thin films (d = 0.27–0.51 μm) spin-coated from chloroform solutions onto glass, is studied. The investigated compounds are polycrystalline (as shown by X-ray Diffraction analysis) and show typical n-type semiconductor behavior. The activation energy of d. c. electric conduction ranges between 1.55 and 2.33 eV. Some correlations between semiconducting characteristics and essential features of molecular structure of organic compounds have been established. In the higher temperature range (400–520 K), the electronic transport properties in present compounds can be explained in the frame of band gap representation model, while in the lower temperature range (300–350 K), the Mott's variable-range hopping conduction model can be conveniently used. - Highlights: • 4,4′-bipyridine and indolizine derivatives in thin films behave as n-type semiconductors. • The electron transfer is favored by extended conjugation and packing capacity. • The band gap representation is suitable in the higher temperature range. • The Mott's VRH conduction model may be used in the lower temperature range.

Hydrolysis of Mg(BH4)2 and its coordination compounds as a way to obtain hydrogen

Science.gov (United States)

Solovev, Mikhail V.; Chashchikhin, Oleg V.; Dorovatovskii, Pavel V.; Khrustalev, Victor N.; Zyubin, A. S.; Zyubina, T. S.; Kravchenko, O. V.; Zaytsev, Alexey A.; Dobrovolsky, Yu. A.

2018-02-01

Three ligand-stabilized Mg(BH4)2-based complexes have been synthesized and evaluated as potential hydrogen storage media for portable fuel cell applications. The new borohydrides: Mg(BH4)2 × 0.5Et2O and Mg(BH4)2 × diglyme (diglyme - CH3O(CH2)2O(CH2)2OCH3) have been synthesized and examined by X-ray single crystal diffraction method. Hydrolysis reactions of the compounds liberate hydrogen in quantities ranging from 46 to 96% of the theoretical yield. The hydrolysis of Mg(BH4)2 and other borohydrides is also accompanied by the diborane formation. The amount of liberated diborane depends on the Mg-coordination environment. To explain this fact quantum-chemical calculations have been performed. It is shown that formation of Mg-O-Mg-bridges enables the side process of diborane generation. It means that the size and denticity of the ligand directly affects the amount of released diborane. In general, the larger the ligand and the higher its denticity, the smaller is amount of diborane produced. The new compound Mg(BH4)2 × diglyme decomposes without diborane formation that allows one to be considered as a new promising chemical hydrogen storage compound for the practical usage.

Comparative catalytic reduction of 4-nitrophenol by polyacrylamide-gold nanocomposite synthesized by hydrothermal autoclaving and conventional heating routes

Science.gov (United States)

Salaheldin, Hosam I.

2017-12-01

Gold nanoparticles (AuNPs) in polymeric polyacrylamide (PAAm) matrix were synthesized using conventional heating and autoclaving thermal techniques. The synthesized Au/PAAm nanocomposite was characterized using UV-vis spectroscopy and high-resolution transmission electron microscopy. The size of the synthesized particles was approximately 6.37 nm and 8.19 nm with the conventional heating and autoclaving thermal techniques, respectively. Electron diffraction x-ray spectroscopy and the Fourier transformation infrared spectroscopy were used for the composition and elemental studies, which confirmed that the Au metallic atoms were synthesized and embedded within a PAAm matrix via a coordination bond between the carbonyl (-CONH2) group and the metallic NPs. X-ray diffraction confirmed the crystalline nature of the fabricated AuNPs with face centered cubic of nanocrystals. The catalytic activity of the as-prepared Au/PAAm nanocomposite for the reduction of 4-nitrophenol to 4-aminophenol was studied in the presence of sodium borohydrate. The synthesized AuNPs had an effective catalytic activity; the smaller NPs synthesized NPs with the conventional heating technique had a higher reaction kinetic rate in comparation with those synthesized with the autoclaving technique. Therefore, the Au/PAAm nanocomposite can be widely used as an eco-friendly, non-toxic, a fast and cost-effective product to remove versatile organic pollutants such as aromatic nitro compounds.

Synthesis and characterization of inverse spinels, intercalation materials for Li-ion batteries

NARCIS (Netherlands)

Van Landschoot, N.

2006-01-01

Chapter 2 describes the solid-state synthesis of LiNiVO4 and LiCoVO4. The materials are prepared at 800C and are phase pure, as shown by X-ray diffraction and have the inverse spinel structure. Due to the solid-state synthesis the particle size is quite large and the particle size distribution is

Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

International Nuclear Information System (INIS)

Rukiah, M.; Assaad, Th.

2012-06-01

The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

Syntheses of 4,6-dihydroxypyrimidine diones, their urease inhibition, in vitro, in silico, and kinetic studies.

Science.gov (United States)

Muhammad, Munira Taj; Khan, Khalid Mohammed; Arshia; Khan, Ajmal; Arshad, Fiza; Fatima, Bibi; Choudhary, M Iqbal; Syed, Naima; Moin, Syed Tarique

2017-12-01

A library of 4,6-dihydroxypyrimidine diones (1-35) were synthesized and evaluated for their urease inhibitory activity. Structure-activity relationships, and mechanism of inhibition were also studied. All compounds were found to be active with IC 50 values between 22.6±1.14-117.4±0.73µM, in comparison to standard, thiourea (IC 50 =21.2±1.3µM). Kinetics studies on the most active compounds 2-7, 16, 17, 28, and 33 were performed to investigate their modes of inhibition, and dissociation constants K i . Compounds 2, 3, 7, 16, 28, and 33 were found to be mixed-type of inhibitors with K i values in the range of 7.91±0.024-13.03±0.013µM, whereas, compounds 4-6, and 17 were found to be non-competitive inhibitors with K i values in the range of 9.28±0.019-13.05±0.023µM. In silico study was also performed, and a good correlation was observed between experimental and docking studies. This study is continuation of our previously reported urease inhibitory activity of pyrimidine diones, representing potential leads for further research as possible treatment of diseases caused by ureolytic bacteria. Copyright © 2017. Published by Elsevier Inc.

Synthesis, electrochemical, spectrophotometric and potentiometric studies of two azo-compounds derived from 4-amino-2-methylquinoline in ethanolic-aqueous buffered solutions

Energy Technology Data Exchange (ETDEWEB)

El-Attar, Mona A.; Ghoneim, Mohamed M. [Analytical Chemistry Research Unit, Chemistry Department, Tanta University (Egypt); Ismail, Iqbal M., E-mail: maema.2011@yahoo.com [Chemistry Department, Faculty of Science, King Abdul Aziz University, Jeddah (Saudi Arabia)

2012-08-15

Two azo-compounds, 2-methyl-4-(5-amino-2-hydroxy-phenylazo)-quinoline (2) and 2-methyl-4-(2-hydroxy-5-nitrophenylazo)-quinoline, derived from 4-amino-2-methylquinoline were synthesized. Their chemical structures were characterized and confirmed by means of elemental chemical analysis, infrared (IR) spectroscopy, {sup 1}H nuclear magnetic resonance (NMR) and mass spectrometry (MS). The electrochemical behavior of the starting compound (4-amino-2-methylquinoline) and of the two synthesized azo-derivatives was studied at the mercury electrode in the B-R universal buffer at various pH values (2-11.5) containing 40% (v/v) ethanol using dc-polarography, cyclic voltammetry and controlled-potential coulometry. Their electrode reaction pathways were elucidated and discussed. The dissociation constants (pKa) of the examined compounds, stability constants and stoichiometry of their complexes in solution with some transition metal ions (Co(II), Ni(II), Cu(II), La(III) and UO{sup 2+}{sub 2}) were determined. (author)

Attempts to Synthesize 3-acyl-4-hydroxycoumarins from Meldrum’s acid -- and Related Chemistry

OpenAIRE

Ye, Fengbin; Tropp, Kristin; Yu, Yiting

2007-01-01

We start our synthetic work with the acylation of Meldrum’s acid to get three different 5-acyl Meldrum’s acids. These compounds are attacked by various nucleophiles containing different hetero atoms to obtain β-ketoesters, β-ketoamides and the corresponding β-keto-phosphorus compounds respectively. New β-ketoamides could be synthesized and characterized. The reaction of acylated Meldrum’s acid and diphenylphosphine did not lead to the expected β-keto-phosphide compound, but the resulting prod...

Syntheses, structures and luminescence for zinc coordination polymers based on a multifunctional 4′-(3-carboxyphenyl)- 3,2′:6′,3″-terpyridine ligand

Energy Technology Data Exchange (ETDEWEB)

Cheng, Yue; Yang, Meng-Lin; Hu, Huai-Ming, E-mail: ChemHu1@NWU.EDU.CN; Xu, Bing; Wang, Xiaofang; Xue, Ganglin

2016-07-15

Six new coordination polymers, [ZnLCl]{sub n}(1), [ZnL{sub 2}]{sub n}·2nH{sub 2}O (2), [Zn{sub 2}L(o-bdc)(OH)]{sub n}·0.5nH{sub 2}O (3), [Zn{sub 2}L(m-bdc)(OH)]{sub n}·nH{sub 2}O (4), [Zn{sub 2}L{sub 2}(p-bdc) (H{sub 2}O){sub 2}]{sub n}·nH{sub 2}O (5), [Zn{sub 2}L(1,2,4-btc)(H{sub 2}O)]{sub n}(6), (HL=4′-(3-carboxyphenyl)- 3,2′:6′,3″-terpyridine, H{sub 2}(o-bdc)= benzene-1,2-dicarboxylic acid, H{sub 2}(m-bdc)= benzene-1,3-dicarboxylic acid, H{sub 2}(p-bdc)= benzene-1,4-dicarboxylic acid, H{sub 3}(1,2,4-btc)= benzene-1,2,4-tricarboxylic acid) have been synthesized under the hydrothermal conditions. Compound 1 displays a 3-connected 2D network structure with point symbol of {8"2.10}. Compound 2 exhibits 1D infinite loop chain structure. Compound 3 possesses a (3,8)-connected 3D framework composed of tetranuclear units with point symbol of {4"3}{sub 2}{4"6.6"1"8.8"4}. Compound 4 features a typical 2D hcb network based on tetranuclear zinc(II) units with point symbol of {4"4.6"2}. Compound 5 presents a classical two-fold penetration sql network with point symbol of {6"3}. Compound 6 can be seen as a (3,3,6)-connected 3D net with point symbol of {4"2.6"4.8"9}{4"2.6}{6"3}. The thermal stability and luminescent properties of compounds 1–6 in the solid state are discussed in detail. - Graphical abstract: Six new Zn(II) coordination polymers based on multicarboxylate and terpyridyl derivative ligands have synthesized under the hydrothermal conditions and the thermal stability and luminescence are discussed. Display Omitted.

Novel Tandem Biotransformation Process for the Biosynthesis of a Novel Compound, 4-(2,3,5,6-Tetramethylpyrazine-1)-4′-Demethylepipodophyllotoxin▿

Science.gov (United States)

Tang, Ya-Jie; Zhao, Wei; Li, Hong-Mei

2011-01-01

According to the structure of podophyllotoxin and its structure-function relationship, a novel tandem biotransformation process was developed for the directional modification of the podophyllotoxin structure to directionally synthesize a novel compound, 4-(2,3,5,6-tetramethylpyrazine-1)-4′-demethylepipodophyllotoxin (4-TMP-DMEP). In this novel tandem biotransformation process, the starting substrate of podophyllotoxin was biotransformed into 4′-demethylepipodophyllotoxin (product 1) with the demethylation of the methoxyl group at the 4′ position by Gibberella fujikuroi SH-f13, which was screened out from Shennongjia prime forest humus soil (Hubei, China). 4′-Demethylepipodophyllotoxin (product 1) was then biotransformed into 4′-demethylpodophyllotoxone (product 2) with the oxidation of the hydroxyl group at the 4 position by Alternaria alternata S-f6, which was screened out from the gathered Dysosma versipellis plants in the Wuhan Botanical Garden, Chinese Academy of Sciences. Finally, 4′-demethylpodophyllotoxone (product 2) and ligustrazine were linked with a transamination reaction to synthesize the target product 4-TMP-DMEP (product 3) by Alternaria alternata S-f6. Compared with podophyllotoxin (i.e., a 50% effective concentration [EC50] of 529 μM), the EC50 of 4-TMP-DMEP against the tumor cell line BGC-823 (i.e., 0.11 μM) was significantly reduced by 5,199 times. Simultaneously, the EC50 of 4-TMP-DMEP against the normal human proximal tubular epithelial cell line HK-2 (i.e., 0.40 μM) was 66 times higher than that of podophyllotoxin (i.e., 0.006 μM). Furthermore, compared with podophyllotoxin (i.e., log P = 0.34), the water solubility of 4-TMP-DMEP (i.e., log P = 0.66) was significantly enhanced by 94%. For the first time, the novel compound 4-TMP-DMEP with superior antitumor activity was directionally synthesized from podophyllotoxin by the novel tandem biotransformation process developed in this work. PMID:21398491

A series of Zn/Cd coordination polymers constructed from 1,4-naphthalenedicarboxylate and N-donor ligands: Syntheses, structures and luminescence sensing of Cr{sup 3+} in aqueous solutions

Energy Technology Data Exchange (ETDEWEB)

Hu, Dong-Cheng [College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Key Laboratory for Preparation and Application of Ordered Structural Materials of Guangdong Province, Shantou University, Shantou 515063 (China); Fan, Yan; Si, Chang-Dai; Wu, Ya-Jun; Dong, Xiu-Yan; Yang, Yun-Xia; Yao, Xiao-Qiang [College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Liu, Jia-Cheng, E-mail: jcliu8@nwnu.edu.cn [College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China)

2016-09-15

A novel series of Zn/Cd coordination polymers based on H{sub 3}L, namely, [Zn{sub 2}(HL){sub 2}(bipy){sub 2}(H{sub 2}O){sub 6}]{sub n} (1), [Zn(HL)(phen)]{sub n} (2), [Cd{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (3), [Zn{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (4) [(H{sub 3}L =4-[(1-carboxynaphthalen-2-yl)oxy]phthalic acid, bipy =4,4′-bipyridine, phen =1,10-phenanthroline, bbi =1,1′-(1,4-butanediyl)bis(imidazole] have been successfully synthesized by solvothermal reaction. Compound 1 possesses two diverse 1D chains constructed by different bipy coligands, which were further connected to form a 3D supramolecular architecture by hydrogen bonding interactions. Compound 2 possesses a complicated 1D chain based on secondary building unit (SBU) with binuclear Zn cluster. Compounds 3 and 4 exhibit similar 2D→3D framework, which can be rationalized as (3,4,4)-connected 3D net with a Schläfli symbol of (6{sup 3}.8.10{sup 2}){sub 2}(6{sup 3}){sub 2}(6{sup 4}.8.10). In particular, compound 3 exhibited a high sensitivity for Cr{sup 3+} in aqueous solutions, which suggest that compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+}. - Graphical abstract: A series of novel Zn/Cd coordination polymers have been successfully synthesized by solvothermal reaction. The unique 3D Cd{sup 2+} polymer containing bbi as second ligand demonstrates high sensitivity for detection of toxic Cr{sup 3+} in aqueous solutions. Display Omitted - Highlights: • π-conjugated semirigid tricarboxylate ligands with naphthalene rings(H{sub 3}L) were rationally designed. • Four Zn/Cd coordination polymers based on H{sub 3}L have been successfully synthesized by solvothermal reaction. • Compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+} with high sensitivity in aqueous solutions.

Development of CXCR4 modulators by virtual HTS of a novel amide-sulfamide compound library.

Science.gov (United States)

Bai, Renren; Shi, Qi; Liang, Zhongxing; Yoon, Younghyoun; Han, Yiran; Feng, Amber; Liu, Shuangping; Oum, Yoonhyeun; Yun, C Chris; Shim, Hyunsuk

2017-01-27

CXCR4 plays a crucial role in recruitment of inflammatory cells to inflammation sites at the beginning of the disease process. Modulating CXCR4 functions presents a new avenue for anti-inflammatory strategies. However, using CXCR4 antagonists for a long term usage presents potential serious side effect due to their stem cell mobilizing property. We have been developing partial CXCR4 antagonists without such property. A new computer-aided drug design program, the FRESH workflow, was used for anti-CXCR4 lead compound discovery and optimization, which coupled both compound library building and CXCR4 docking screens in one campaign. Based on the designed parent framework, 30 prioritized amide-sulfamide structures were obtained after systemic filtering and docking screening. Twelve compounds were prepared from the top-30 list. Most synthesized compounds exhibited good to excellent binding affinity to CXCR4. Compounds Ig and Im demonstrated notable in vivo suppressive activity against xylene-induced mouse ear inflammation (with 56% and 54% inhibition). Western blot analyses revealed that Ig significantly blocked CXCR4/CXCL12-mediated phosphorylation of Akt. Moreover, Ig attenuated the amount of TNF-α secreted by pathogenic E. coli-infected macrophages. More importantly, Ig had no observable cytotoxicity. Our results demonstrated that FRESH virtual high throughput screening program of targeted chemical class could successfully find potent lead compounds, and the amide-sulfamide pharmacophore was a novel and effective framework blocking CXCR4 function. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Synthesis and antimicrobial screening of novel 2-(5-(4-(allyloxy-3-methoxyphenyl-1H-pyrazol-3-ylphenols analogues of 2-(4-(allyloxy-3-methoxyphenyl-4H-chromen-4-ones

Directory of Open Access Journals (Sweden)

Asha V. Chate

2012-01-01

Full Text Available A series of novel 2-(5-(4-(allyloxy-3-methoxyphenyl-1H-pyrazol-3-ylphenols derivatives have been synthesized via the ring opening of 2-(4-(allyloxy-3-methoxyphenyl-4H-chromen-4-ones in ethanol and hydrazine hydrate under reflux condition. The synthesized compounds were screened for antibacterial and antifungal activity against bacteria Staphylococcus aureus (MRSA E710 and Escherichia coli (ATCC 25922 and fungi Candida albicans and Aspergillus fumigates respectively. Some of the tested compounds showed significant antimicrobial activity. 1H NMR, IR, Mass spectral data and elemental analysis elucidated the structures of the all newly synthesized compounds.

New vanadium tellurites: Syntheses, structures, optical properties of noncentrosymmetric VTeO{sub 4}(OH), centrosymmetric Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})

Energy Technology Data Exchange (ETDEWEB)

Liang, Ming-Li [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350108 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Marsh, Matthew [Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States); Shang, Xian-Xing [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350108 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Mao, Jiang-Gao [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Albrecht-Schmitt, Thomas E. [Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States); Kong, Fang, E-mail: kongfang@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States)

2017-05-15

Two new vanadium tellurites, VTeO{sub 4}(OH) (1) and Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2), have been synthesized successfully with the use of hydrothermal reactions. The crystal structures of the two compounds were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the polar space group Pca2{sub 1} (No. 29) while compound 2 crystallizes in the centrosymmetric space group C2/c (No. 15). The topography of compound 1 reveals a two-dimensional, layered structure comprised of VO{sub 6} octahedral chains and TeO{sub 3}(OH) zig-zag chains. Compound 2, on the contrary, features a three-dimensional [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})]{sup 4-} anionic framework with Ba{sup 2+} ions filled into the 10-member ring helical tunnels. The [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})]{sup 4-} anionic network is the first 3D vanadium tellurite framework to be discovered in the alkaline-earth vanadium tellurite system. Powder second harmonic generation (SHG) measurements indicate that compound 1 shows a weak SHG response of about 0.3×KDP (KH{sub 2}PO{sub 4}) under 1064 nm laser radiation. Infrared spectroscopy, elemental analysis, thermal analysis, and dipole moment calculations have also been carried out. - Graphical abstract: VTeO{sub 4}(OH) (1) crystallizes in the noncentrosymmetric space group Pca2{sub 1} (No. 29) while Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) crystallizes in the centrosymmetric space group C2/c (No. 15). - Highlights: • VTeO{sub 4}(OH) (1) and Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) have been synthesized successfully with the use of hydrothermal reactions. • VTeO{sub 4}(OH) (1) crystallizes in the noncentrosymmetric space group Pca2{sub 1} and displays a weak SHG response. • VTeO{sub 4}(OH) (1) represents only the fourth SHG-active material found in vanadium tellurite systems. • Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) exhibits a novel three-dimensional [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10

SYNTHESIS, CHARACTERIZATION AND ANTIOXIDANT ACTIVITIES OF NOVEL 1-(MORPHOLINE-4-YL-METHYL-3-ALKYL(ARYL-4-[4-(DIMETHYLAMINO-BENZYLIDENAMINO]-4,5-DIHYDRO-1H-1,2,4-TRIAZOL-5-ONES

Directory of Open Access Journals (Sweden)

Özlem Gürsoy Kol

2016-08-01

Full Text Available In this paper, eight novel 1-(morpholine-4-yl-methyl-3-alkyl(aryl-4-[4-(dimethylamino-benzylidenamino]-4,5-dihydro-1H-1,2,4-triazol-5-ones (2 were obtained by the reactions of 3-alkyl(aryl-4-[4-(dimethylamino-benzylidenamino]-4,5-dihydro-1H-1,2,4-triazol-5-ones (1 with formaldehyde and morpholine. The novel synthesized compounds were identified by IR, 1H NMR and 13C NMR spectral data. Besides, the newly synthesized compounds were analysed for their in vitro potential antioxidant capacities in three different assays. All of the compounds demonstrated significant activity for metal chelating effect.

Antioxidant Activity of Novel Fused Heterocyclic Compounds Derived from Tetrahydropyrimidine Derivative.

Science.gov (United States)

Salem, Marwa Sayed; Farhat, Mahmoud; Errayes, Asma Omar; Madkour, Hassan Mohamed Fawzy

2015-01-01

6-(Benzo[d][1,3]dioxol-5-yl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile has been utilized for synthesis of the fused heterocyclic compounds namely thiazolopyrimidines, tetrazolopyrimidine, pyrimidoquinazoline, pyrimidothiazolopyrimidine, pyrimidothiazolotriazine and pyrrolothiazolopyrimidine derivatives. The newly synthesized compounds were characterized by IR, (1)H-NMR, (13)C-NMR, and mass spectral data. Antioxidant activities of all synthesized compounds were investigated.

Synthesis, Characterization and Antifungal Evaluation of 5-Substituted-4-Amino-1,2,4-Triazole-3-Thioesters

Directory of Open Access Journals (Sweden)

Aurangzeb Hasan

2011-01-01

Full Text Available A series of 5-substituted-4-amino-1,2,4-triazole-3-thioesters was synthesized by converting variously substituted organic acids successively into the corresponding esters, hydrazides, 5-substituted-1,3,4-oxadiazole-2-thiols, 5-substituted-1,2,4-triazole-2-thiols and 5-substituted-1,3,4-oxadiazole-2-thioesters. Finally the target compounds were obtained by refluxing 5-substituted-1,3,4-oxadiazole-2-thioesters in the presence of hydrazine hydrate and absolute alcohol. The structures of the synthesized compounds were established by physicochemical and spectroscopic methods. The synthesized compounds were evaluated for their in vitro antifungal activity. Some of the evaluated compounds possessed significant antifungal activity as compared to a terbinafine standard.

Syntheses, structures, and magnetic properties of three new MnII-[MoIII(CN)7]4- molecular magnets.

Science.gov (United States)

Wei, Xiao-Qin; Pi, Qian; Shen, Fu-Xing; Shao, Dong; Wei, Hai-Yan; Wang, Xin-Yi

2018-05-22

By reaction of K4[MoIII(CN)7]·2H2O, Mn(ClO4)2·6H2O and bidentate chelating ligands, three new cyano-bridged compounds, namely Mn2(3-pypz)(H2O)(CH3CN)[Mo(CN)7] (1), Mn2(1-pypz)(H2O)(CH3CN)[Mo(CN)7] (2) and Mn2(pyim)(H2O)(CH3CN)[Mo(CN)7] (3) (3-pypz = 2-(1H-pyrazol-3-yl)pyridine, 1-pypz = 2-(1H-pyrazol-1-yl)pyridine, pyim = 2-(1H-imidazol-2-yl)pyridine), have been synthesized and characterized structurally and magnetically. Single crystal X-ray analyses revealed that although the chelating ligands are different, compounds 1 to 3 are isomorphous and crystallize in the same monoclinic space group C2/m. Connected by the bridging cyano groups, one crystallographically unique [Mo(CN)7]4- unit and three crystallographically unique MnII ions of different coordination environments form similar three-dimensional frameworks, which have a four-nodal 3,4,4,7-connecting topological net with a vertex symbol of {43}{44·62}2{410·611}. Magnetic measurements revealed that compounds 1-3 display long-range magnetic ordering with critical temperatures of 64, 66 and 62 K, respectively. These compounds are rare examples of a small number of chelating co-ligand coordinated [Mo(CN)7]4--based magnetic materials. Specifically, the bidentate chelating ligands were successfully introduced into the heptacyanomolybdate system for the first time.

Syntheses and structures of three f-element selenite/hydroselenite compounds

International Nuclear Information System (INIS)

Burns, Wendy L.; Ibers, James A.

2009-01-01

The selenite/hydroselenite compounds Ce(SeO 3 )(HSeO 3 ), Tb(SeO 3 )(HSeO 3 ).2H 2 O, and Cs[U(SeO 3 )(HSeO 3 )].3H 2 O were synthesized by hydrothermal means at 453 K from the reaction of CeO 2 or Tb 4 O 7 or UO 2 with SeO 2 and CsCl (as a mineralizer). Ce(SeO 3 )(HSeO 3 ) crystallizes in the non-centrosymmetric orthorhombic space group Pca2 1 . The structure comprises a two-dimensional network of interconnected CeO 10 bicapped distorted square antiprisms and SeO 3 trigonal pyramids. Tb(SeO 3 )(HSeO 3 ).2H 2 O crystallizes in the non-centrosymmetric orthorhombic space group P2 1 2 1 2 1 . The structure features a two-dimensional layer of interconnected TbO 8 distorted square antiprisms and SeO 3 trigonal pyramids. Cs[U(SeO 3 )(HSeO 3 )].3H 2 O crystallizes in the centrosymmetric monoclinic space group P2 1 /n. The structure consists of two-dimensional layers of interconnected UO 7 pentagonal bipyramids and SeO 3 trigonal pyramids. The layers in all three structures are held together by hydrogen-bonding networks. - Graphical abstract: Structure of Ce[U(SeO 3 )(HSeO 3 )].3H 2 O (Cs, purple; U, black; Se, blue; O, red; O w , green; H, gray).

Syntheses, Crystal Structures, Magnetic Behaviours, and Thermal Properties of Three Hydrogen-Bonding Networks Containing Dicyanamide and 4-Hydroxypyridine

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Lingling Zheng

2013-01-01

Full Text Available Three new dicyanamide-bridged polymeric complexes of {[Mn(dca2(L2]·2H2O}n (1, {[Cd(dca2(L2]·2H2O}n (2, and {[Co(dca2(L2]2(L}n (3 (dca = dicyanamide, L = pyridinium-4-olate have been synthesized and structurally characterized. In the three compounds, the protons of hydroxyl groups of 4-hydroxypyridine transfer to pyridyl nitrogen atoms. Compounds 1 and 2 are isomorphous forming one-dimensional [M(dca2(L2]n chains where metals are connected by double dca anions. These one-dimensional chains are extended into two-dimensional layers through weak C–H⋯N hydrogen bonds. Further, these layers are assembled into a three-dimensional supramolecular network through N–H⋯O, O–H⋯O hydrogen bonds. Complex 3 is a coordination layer of (4, 4 topology with octahedral metal centers linked by four single μ1,5-bridges. These layers are interlocked by N–H⋯O, O–H⋯O hydrogen bonds from coordinated water molecules and free L molecules, which leads to a three-dimensional supramolecular architecture. The variable temperature magnetic susceptibilities measurement of compounds 1 and 3 shows the existence of weak antiferromagnetic interactions between the metal centers. The thermogravimetric analyses of the compounds 1–3 are also discussed.

Synthesis and antibacterial activity of novel Pyrazolo [3, 4-B] quinoline based heterocyclic azo compounds and their dyeing performance

International Nuclear Information System (INIS)

Thaokar, Sanjay F.; Patel, Dinesh M.; Patel, Manish P.; Patel, Ranjan G.

2007-01-01

3-Amino-6-methyl-1H- pyrazolo [3, 4-B] quinoline was synthesized in good yield. Monoazo compounds were prepared using this intermediate as diazo component with various heterocyclic coupling components. All the azo compounds were characterized by their percentage yield, melting point, elemental analysis, UV-visible spectra, IR-spectra and dyeing performance on nylon and polyester fibres and by their antibacterial activity against gram positive and gram negative bacteria. (author)

Magnetic and photocatalytic studies on Zn1-xMgxFe2O4 nanocolloids synthesized by solvothermal reflux method.

Science.gov (United States)

Manohar, A; Krishnamoorthi, C

2017-12-01

Biocompatible magnetic semiconductor Zn 1-x Mg x Fe 2 O 4 (x=0, 0.1, 0.3, 0.5 & 0.7) nanoparticles of around 10nm diameter were synthesized by solvothermal reflux method. The method produces well separated and narrow size distributed nanoparticles. Crystal structure, morphology, particles surface properties, surfactant quantity, colloidal stability, magnetic properties and photocatalytic properties of the synthesized nanoparticles were studied. Different characterizations confirmed that all compounds were single crystals and superparamagnetic at room temperature. Saturation mass magnetization (M s =57.5emu/g) enhances with substituent Mg 2+ concentration due to promotion of mixed spinel (normal and inverse) structure. Photocatalytic activity of all synthesized magnetic semiconductor nanoparticles were studied through methylene blue degradation. The degradation of 98% methylene blue was observed on 60 min irradiation of light. It is observed that photocatalytic activity slightly enhances with substituent Mg 2+ concentration. The synthesized biocompatible magnetic semiconductor nanoparticles can be utilized as photocatalysts and could also be recycled and separated by applying an external magnetic field. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis, urease inhibition, antioxidant and antibacterial studies of some 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones and their 3,6-disubstituted 1,2,4-triazolo[3,4-b]1,3,4-thiadiazole derivatives

International Nuclear Information System (INIS)

Hanif, Muhammad; Saleem, Muhammad; Rama, Nasim Hasan; Hussain, Muhammad Tahir; Zaib, Sumera; Aslam, Muhammad Adil M.; Iqbal, Jamshed; Jones, Peter G.

2012-01-01

A new series of 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones, bearing various methoxybenzyl- and methoxyphenethyl groups, was synthesized by refluxing potassium hydrazinecarbodithioate salts in dilute aqueous solution of hydrazine hydrate. These salts were formed by the reaction of acid hydrazides and carbon disulfide in methanolic potassium hydroxide solution at 0-5 deg C. 4-Amino- 5-aryl-3H-1,2,4-triazole-3-thiones were condensed with different substituted aromatic acids to yield 3,6-disubstituted-1,2,4-triazolo[3,4-b]1,3,4-thiadiazoles. The structures of the synthesized compounds were characterized by infrared (IR), 1 H and 13 C nuclear magnetic resonance (NMR), elemental analysis and mass spectrometric (MS) studies. All the synthesized compounds were screened for their urease inhibition, antioxidant and antibacterial activities. Some compounds showed excellent urease inhibition activity, more than the standard drug. Others exhibited potent antioxidant activity. All the compounds showed significant antibacterial activities as compared to the standard drug. (author)

Synthesis and antimalarial activity evaluation of 3-(3-(7-chloroquinolin-4-ylaminopropyl-1,3-thiazinan-4-one derivatives

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Mukesh Kumar Kumawat

2016-09-01

Full Text Available Some novel derivatives of 3-(3-(7-chloroquinolin-4-ylaminopropyl-1,3-thiazinan-4-one were synthesized and characterized by their physical and spectral data. All the synthesized compounds were subsequently screened for in vitro antimalarial activity against chloroquine sensitive strain of Plasmodium falciparum (RKL-2 employing chloroquine as the reference drug. Most of the synthesized compounds exhibited mild to moderate susceptibilities towards the parasite in comparison to the standard. It was found that antimalarial activity of 3-(3-(7-chloroquinolin-4-ylaminopropyl-2-(4-bromophenyl-1,3-thiazinan-4-one was marginally superior than all the compounds evaluated.

Syntheses and structures of three supramolecular complexes based on 2-(pyridine-2-yl)-1H-imidazole-4,5-dicarboxylic acid

Science.gov (United States)

Yu, Xiao-Yang; Zhang, Xiao; Liu, Zhi-Gang; Cui, Xiao-Bing; Xu, Jia-Ning; Luo, Yu-Hui

2017-11-01

Three new supramolecular compounds, [Cu(o-HPIDC)(bpy)(H2O)]·2H2O 1, [Cu(o-H2PIDC)(phen)Cl]·[Cu(phen)2Cl]·10H2O·Cl 2 and {[Cd(o-H2PIDC)(H2O)2Cl]·H2O}23 (o-H3PIDC = 2-(pyridine-2-yl)-1H-imidazole-4,5-dicarboxylic acid, bpy = 2,2'-bipyridine, phen = 1,10-phenanthroline), were hydrothermally synthesized and characterized. In compound 1, the adjacent two supramolecular layers are constructed from different types of helical chains with the same pitch. In compound 2, the adjacent 2D water-chloride layers, {[(H2O)10Cl]-}n, are pillared by [Cu(o-H2PIDC)(phen)Cl] units to form the overall 3D supramolecular network with 1D channels through Osbnd H⋯O hydrogen bond interactions. In compound 3, two Cd(II) are linked into a binuclear [Cd2(o-H2PIDC)2(H2O)4Cl2] with a ten-membered ring by two o-H2PIDC- ligands. The three compounds self-assemble into 3D supramolecular structures via hydrogen bond and π-π stacking interactions. The fluorescence properties of compound 3 was also investigated.

Syntheses, crystal structures and properties of series of 4d–4f ln(III)–Ag(I) heterometallic coordination polymers

Energy Technology Data Exchange (ETDEWEB)

Ran, Xing-Rui [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Wang, Ning [School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore); Xie, Wei-Ping; Xiong, Yan-Ju; Cheng, Qian [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Long, Yi [School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 (Singapore); Yue, Shan-Tang, E-mail: yuesht@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, Guangzhou (China); Liu, Ying-Liang [College of Science, South China Agricultural University, Guangzhou 510642 (China)

2015-05-15

By control of the experimental parameters such as ligands, pH value and reacting temperature, series of three-dimensional (3D) 4d–4f Ln(III)–Ag(I) porous coordination polymers (PCPs) with interesting chain-layer construction, namely, ([Ln{sup III}Ag{sup I}(na)(ina)(ox)]·2(H{sub 2}O)){sub n} [Ln=Sm(1), Eu(2), Gd(3), Tb(4), Dy(5), Ho(6), Y(7), Yb(8)], have been successfully synthesized under hydrothermal conditions and structurally characterized. All the complexes are characterized by elemental analyses, FT-IR spectroscopy, Powder X-ray diffraction (PXRD) and thermogravimetric analyses (TGA). Furthermore, the luminescence properties of compounds 2 and 4 and the magsnetic properties of complexes 3 and 5 were also investigated in detail. - Graphical abstract: Series of three-dimensional (3D) 4d–4f Ln(III)–Ag(I) porous coordination polymers (PCPs) with interesting chain-layer construction which are featured by tetranuclear Ln{sub 2}Ag{sub 2} and ‘non-linear’ N–Ag–N linkages. - Highlights: • Complexes 1–8 are first built by three kinds of organic ligands based on nicotinic acid and isonicotinic acid. • PCPs 1–8 are featured by tetranuclear Ln{sub 2}Ag{sub 2} and ‘non-linear’ N–Ag–N linkages. • The total solvent-accessible volume of PCP 2 comprises 11.6% of the crystal volume after dislodging the free water molecules. • Complexes 2 and 4 exhibit characteristic lanthanide-centered luminescence, while compounds 3 and 5 show antiferromagnetic behaviors.

Synthesis of 1-Substituted-4-(Pyridin-4-yl)

African Journals Online (AJOL)

Purpose: To synthesize a new series of 1-substituted-4-(pyridin-4-yl) [1,2,4] triazolo [4,3-a]quinazolin- 5(4H)-ones and evaluate them for H1-antihistaminic activity with negligible side effects in guinea pigs. Methods: The synthesized compounds were characterized by Infrared spectroscopy (IR), proton nuclear magnetic ...

Fast-Rate Capable Electrode Material with Higher Energy Density than LiFePO4: 4.2V LiVPO4F Synthesized by Scalable Single-Step Solid-State Reaction.

Science.gov (United States)

Kim, Minkyung; Lee, Seongsu; Kang, Byoungwoo

2016-03-01

Use of compounds that contain fluorine (F) as electrode materials in lithium ion batteries has been considered, but synthesizing single-phase samples of these compounds is a difficult task. Here, it is demonstrated that a simple scalable single-step solid-state process with additional fluorine source can obtain highly pure LiVPO 4 F. The resulting material with submicron particles achieves very high rate capability ≈100 mAh g -1 at 60 C-rate (1-min discharge) and even at 200 C-rate (18 s discharge). It retains superior capacity, ≈120 mAh g -1 at 10 C charge/10 C discharge rate (6-min) for 500 cycles with >95% retention efficiency. Furthermore, LiVPO 4 F shows low polarization even at high rates leading to higher operating potential >3.45 V (≈3.6 V at 60 C-rate), so it achieves high energy density. It is demonstrated for the first time that highly pure LiVPO 4 F can achieve high power capability comparable to LiFePO 4 and much higher energy density (≈521 Wh g -1 at 20 C-rate) than LiFePO 4 even without nanostructured particles. LiVPO 4 F can be a real substitute of LiFePO 4.

Synthesis and Application of Polymeric Fluorescent Compounds Based on Coumarin

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Guojun Liu

2015-06-01

Full Text Available In this work, a multifunctional yellowing inhibitor was synthesized by the Pechmann method. In order to obtain the target compound, 7-hydroxy-4-methyl coumarin was prepared by using the raw materials of resorcinol and ethyl acetoacetate, with toluene-p-sulfonic acid as the catalyst. New polymeric fluorescent compounds were synthesized by connecting the 7-hydroxy-4-methyl coumarin, the hindered amine light stabilizer 4-amion-2,2,6,6-tetramentylniperidine, and a series of polyethylene glycol segments into the same molecule with cyanuric chloride as a bridge. The structures of the synthesized molecules were confirmed by FT-IR, 1H NMR, and elemental analysis. The luminescent properties of the fluorescent compounds were studied by UV-vis spectroscopy and fluorescence spectroscopy. The integration effect between the fluorescent compounds and paper was tested by a scanning electron microscope. The light stability effect on the paper sheet was tested using an ultraviolet aging apparatus. The results indicate that the polymeric fluorescent compounds had a positive effect on the light stability of the high-yield pulp.

Microwave assistant synthesis, crystal structure and biological activity of a 1,2,4-triazole compound

International Nuclear Information System (INIS)

Ke, W.; Sun, N.B.

2013-01-01

The title compound (C/sub 17/H/sub 14/F/sub 2/N/sub 4/SO) were synthesized and recrystallized from CH/sub 3/CN. The compound was characterized by 1h-nmr, ftir, ms, hrms and x-ray diffraction. the compound crystallized in the monoclinic space group c2/c with a = 27.532(6), b 8.9596(18), c 14.609(3) alpha = 90, beta = 112.59(3), lambda =90 degree, gamma = 3327.1(12) alpha 3, z = 8 and r = 0.0327 for 2596 observed reflections with 1 > 2 (i). x-ray analysis reveals that not only intermolecular N-H-N interactions, but also C-H Pie stacking interactions exist in the adjacent molecules. The biological activities results showed that it exhibited significant herbicidal activity towards brassica napus. (author)

Synthesis, Crystal and Electronic Structure of the Quaternary Magnetic EuTAl4Si2 (T = Rh and Ir) Compounds

Energy Technology Data Exchange (ETDEWEB)

Maurya, Arvind [Tata Institute of Fundamental Research; Thamizhavel, Arumugam [Tata Institute of Fundamental Research; Provino, Alessia [University of Genova; Pani, Marcella [University of Genova; Manfrinetti, Pietro [University of Genova; Paudyal, Durga [Ames Laboratory; Dhar, Sudesh Kumar [Tata Institute of Fundamental Research

2014-01-22

Single crystals of the quaternary europium compounds EuRhAl4Si2 and EuIrAl4Si2 were synthesized by using the Al–Si binary eutectic as a flux. The structure of the two quaternary compounds has been refined by single crystal X-ray diffraction. Both compounds are stoichiometric and adopt an ordered derivative of the ternary KCu4S3 structure type (tetragonal tP8, P4/mmm). The two compounds reported here represent the first example of a quaternary and truly stoichiometric 1:1:4:2 phase crystallizing with this structure type. In light of our present results, the structure of the BaMg4Si3 compound given in literature as representing a new prototype is actually isotypic with the KCu4S3 structure. Local spin density approximation including the Hubbard U parameter (LSDA + U) calculations show that Eu ions are in the divalent state, with a significant hybridization between the Eu 5d, Rh (Ir) 4d (5d), Si 3p and Al 3p states. Magnetic susceptibility measured along the [001] direction confirms the divalent nature of the Eu ions in EuRhAl4Si2 and EuIrAl4Si2, which order magnetically near 11 and 15 K, respectively.

Syntheses, Characterization, Resolution, and Biological Studies of Coordination Compounds of Aspartic Acid and Glycine

Science.gov (United States)

Akinkunmi, Ezekiel; Ojo, Isaac; Adebajo, Clement; Isabirye, David

2017-01-01

Enantiomerically enriched coordination compounds of aspartic acid and racemic mixtures of coordination compounds of glycine metal-ligand ratio 1 : 3 were synthesized and characterized using infrared and UV-Vis spectrophotometric techniques and magnetic susceptibility measurements. Five of the complexes were resolved using (+)-cis-dichlorobis(ethylenediamine)cobalt(III) chloride, (+)-bis(glycinato)(1,10-phenanthroline)cobalt(III) chloride, and (+)-tris(1,10-phenanthroline)nickel(II) chloride as resolving agents. The antimicrobial and cytotoxic activities of these complexes were then determined. The results obtained indicated that aspartic acid and glycine coordinated in a bidentate fashion. The enantiomeric purity of the compounds was in the range of 22.10–32.10%, with (+)-cis-dichlorobis(ethylenediamine)cobalt(III) complex as the more efficient resolving agent. The resolved complexes exhibited better activity in some cases compared to the parent complexes for both biological activities. It was therefore inferred that although the increase in the lipophilicity of the complexes may assist in the permeability of the complexes through the cell membrane of the pathogens, the enantiomeric purity of the complexes is also of importance in their activity as antimicrobial and cytotoxic agents. PMID:28293149

Synthesis and Herbicidal Activities of Novel 4-(4-(5-methyl-3-arylisoxazol-4-ylthiazol-2-ylpiperidyl Carboxamides and Thiocarboxamides

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Ai-Dong Zhang

2009-03-01

Full Text Available A series of novel 4-(4-(5-methyl-3-arylisoxazol-4-ylthiazol-2-ylpiperidyl carboxamides and thiocarboxamides were synthesized as potential lead compounds of inhibitors targeting D1 protease in plants. These compounds were designed on the basis of a D1 protease inhibitor hit structure identified by homology modeling and virtual screening. The syntheses of these compounds were accomplished via a four-step procedure including the isoxazole ring formation, a-bromination of acetyl group, thiazole ring formation, and carboxamide/thiocarboxamide attachment. The in vivo herbicidal activity tests show that most compounds possess moderate to good herbicidal activities. The enzyme activity of one compound against the native spinach D1 protease exhibits a competitive inhibition. The results suggest that these compounds are indeed potential inhibitors for targeting D1 protease in plants.

A new three-dimensional cobalt phosphate: Co5(OH2)4(HPO4)2(PO4)2

International Nuclear Information System (INIS)

Han Zhangang; Tian Aixiang; Peng Jun; Zhai Xueliang

2006-01-01

A three-dimensional (3D) cobalt phosphate: Co 5 (OH 2 ) 4 (HPO 4 ) 2 (PO 4 ) 2 (1), has been synthesized by hydrothermal reaction and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic techniques. The title compound is a template free cobalt phosphate. Compound 1 exhibits a complex net architecture based on edge- and corner-sharing of CoO 6 and PO 4 polyhedra. The magnetic susceptibility measurements indicated that the title compound obeys Curie-Weiss behavior down to a temperature of 17 K at which an antiferromagnetic phase transition occurs. - Graphical abstract: A 3D cobalt phosphate with a neutral framework: Co 5 (OH 2 ) 4 (HPO 4 ) 2 (PO 4 ) 2 (1), has been synthesized and characterized. Compound 1 exhibits a complex net architecture based on edge- and corner-sharing of CoO 6 and PO 4 polyhedra. Its magnetic property was researched

Syntheses of New Unsymmetrical and Symmetrical Diarylsulphides and Diarylsulphones Containing Thiazolinyl and Thiazolidinonyl Moieties Using 4,4'-Diacetyldiphenylsulphide

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M. I. Abdel-Monem

2003-07-01

Full Text Available Condensation of 4,4’-diacetyldiphenyl sulphide (2 with variable amounts of thiosemicarbazide (3 in refluxing ethanol and in the presence of catalytic amounts of dry piperidine afforded only 4-acetylthiosemicarbazone-4’-acetyldiphenyl sulphide (5. Condensation of 2 with excess semicarbazide hydrochloride (4 in the presence of fused sodium acetate and/or piperidine yielded 4,4’-diacetylsemicarbazone diphenyl sulphide (6, whereas use of equimolar amounts of 2 and 4 afforded 4-acetyl-semicarbazone-4’-acetyldiphenyl sulphide (7. 4-Acetylsemicarbazone-4’-acetylthiosemicarbazone diphenyl sulphide (8 was also obtained via two different routes. The effect of tautomeric structure 5d is discussed. 4-(4"-phenyl-Δ3-thiazoline-2"-acetylazino-4’-acetyldiphenyl sulphide (9, 4-(5"-carboxyethyl-4"-thiazolidinone-2"-acetylazino-4’-acetyldiphenyl sulphide (10, 4-(4"-thiazolidinone-2’-acetylazino-4’-acetyldiphenyl sulphide (11 and 4-(4"-methyl-Δ3-thiazoline-2"-acetylazino-4’-acetyldiphenyl sulphide (12 were prepared by interaction of 5 with phenacylbromide, bromodiethylmalonate, chloro ethylacetate and chloroacetone, respectively. Sulphides 9-12 were easily condensed with 3 to afford the corresponding 4-(heterocyclic moiety-2"-acetylazino-4’-acetylthiosemicarbazone diphenyl sulphides 23-26. Oxidation of the prepared sulphides 5-7, 9-12, 23 and 25-26 using H2O2/glacial AcOH mixtures yielded only 4,4’-diacetyldiphenyl sulphone (13 as the main product in every case, besides 3 and 4 in certain cases. Unsymmetrical and symmetrical sulphones 14-22 were obtained starting from 13. The structures of the synthesized compounds are based on IR, 1H-NMR, 13C-NMR and mass spectral data. A theoretical study on some of the prepared compounds using molecular modeling was carried out.

Syntheses and pyrolytic studies of salicylate derivatives of ...

African Journals Online (AJOL)

New salicylate derivatives of heteronucleic-μ-oxoisopropoxide [SnO2AlB(OPri)4] have been synthesized by the thermal condensation of μ-oxoisopropoxide and methyl/ethyl/phenyl/phenyl ethyl salicylates in different molar ratios (1:1-1:2) yielding the compounds of the type [SnO2AlB(OPri)4-n(RSAL)n] (where n is 1-2 and ...

Microanalysis on CuInSe2 compound synthesized by mechanochemical processing

International Nuclear Information System (INIS)

Wu Sumei; Xue Yuzhi; Zhang Zhihua

2010-01-01

CuInSe 2 (CIS) compound has been synthesized by mechanochemical processing (MCP) with different process parameters. The effect of milling time and different molar ratios of Cu:In:Se was investigated. The obtained materials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) for evaluating their crystal structure, grain size, morphology and composition. Field emission transmission electron microscopy (FETEM) was used to detect the smog particles produced during the milling. The results revealed that the obtained powder was chalcopyrite CuInSe 2 and the particle size was smaller than 5 μm after milling for 60 min. The EDS analysis indicated that the smog was volatile selenium. The composition of the products deviated from those of starting materials after MCP. The mechanism about mechanically induced self-propagating reaction which occurred during milling copper, indium and selenium powders was also discussed.

Oxidative stress protection by newly synthesized nitrogen compounds with pharmacological potential.

Science.gov (United States)

Silva, João P; Areias, Filipe M; Proença, Fernanda M; Coutinho, Olga P

2006-02-09

In this study we used new nitrogen compounds obtained by organic synthesis whose structure predicted an antioxidant potential and then an eventual development as molecules of pharmacological interest in diseases involving oxidative stress. The compounds, identified as FMA4, FMA5, FMA7 and FMA8 differ in the presence of hydroxyl groups located in the C-3 and/or C-4 position of a phenolic unit, which is possibly responsible for their free radicals' buffering capacity. Data from the DPPH discoloration method confirm the high antiradical efficiency of the compounds. The results obtained with cellular models (L929 and PC12) show that they are not toxic and really protect from membrane lipid peroxidation induced by the ascorbate-iron oxidant pair. The level of protection correlates with the drug's lipophilic profile and is sometimes superior to trolox and equivalent to that observed for alpha-tocopherol. The compounds FMA4 and FMA7 present also a high protection from cell death evaluated in the presence of a staurosporine apoptotic stimulus. That protection results in a significant reduction of caspase-3 activity induced by staurosporine which by its turn seems to result from a protection observed in the membrane receptor pathway (caspase-8) together with a protection observed in the mitochondrial pathway (caspase-9). Taken together the results obtained with the new compounds, with linear chains, open up perspectives for their use as therapeutical agents, namely as antioxidants and protectors of apoptotic pathways. On the other hand the slight pro-oxidant profile obtained with the cyclic structures suggests a different therapeutic potential that is under current investigation.

Synthesis, structure and two-photon absorption properties of a new multi-branched compound, 1,2,4,5-tetrakis(4-pyridylvinyl)benzene

International Nuclear Information System (INIS)

Wang Lei; Tao Xutang; Yang Jiaxiang; Yu Wentao; Ren Yan; Xin Qian; Liu Zhi; Jiang Minhua

2004-01-01

A conjugated and symmetric multi-branched compound, 1,2,4,5-tetrakis(4-pyridylvinyl)benzene (TKPVB), has been synthesized and the crystal structures of TKPVB and its intermediate, 1,2,4,5-tetrakis(dimethoxyphosphorylmethyl)benzene, were determined by diffraction method. TKPVB with four units of 4-vinylpyridine moieties attached to the central benzene core presents an A-π-A general framework, where A is a π-deficient pyridine ring. The single-photon and two-photon absorption and fluorescence properties in different solvents of varying polarity have been investigated. It is also found that the one- and two-photon-induced fluorescence spectra are quite similar, which indicate that the one- and two-photon allowed-excited states are the same

Heme polymerization inhibition activity (HPIA) assay of synthesized xanthone derivative as antimalarial compound

Science.gov (United States)

Fitriastuti, Dhina; Jumina, Priatmoko

2017-03-01

Xanthone is a phenolic secondary metabolite of Garcinia and Calophyllum herbs which has been clinically proven to display anti malaria activity. In the present paper, 2,3,4-trihydroxy-5-methyl xanthone which has been synthesized from gallic acid and o-cresol in Eaton's reagent was tested for its activity as antimalarial. Thus, HPIA assay of the synthesized xanthones was successfully conducted. The HPIA assay was carried out towards the xanthone, chloroquine diphosphate as positive control and distilled water as negative control in various concentration. The samples were reacted with hematin (ferriprotoporphyrin IX hydroxide) and the absorbance of the precipitate was observed by using Elisa reader. The results of HPIA assay showed that 2,3,4-trihydroxy-5-methyl xanthone and chloroquine have IC50 values of 0.755 and 1.462 mg/mL or 2.92 and 4.57 mM, respectively. 2,3,4-Trihydroxy-5-methyl xanthone displayed better antimalarial activity than chloroquine.

Synthesis of Novel p-tert-Butylcalix[4]arene Derivative: Structural Characterization of a Methanol Inclusion Compound

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Silvana Moris

2016-09-01

Full Text Available A p-tertbutylcalix[4]arene derivative was synthesized from a reaction of the diisothiocyanate p-tertbutylcalix[4]arene, obtaining crystals that were then characterized by mass spectroscopy, Raman spectroscopy, and single-crystal X-ray diffraction. The molecule presents two acid carbamothioic-n-ethoxy-methyl-ester substituent groups. Through crystallization of this compound, it was also found that it includes a methanol molecule within the aromatic cavity. The inclusion of the methanol molecule is due to favorable CH∙∙∙π interactions.

Formation and magnetic properties of compounds Er(Fe1-xCox)11.35Nb0.65 (0≤x≤0.4)

International Nuclear Information System (INIS)

Wang, K.-Y.; Chen, D.-X.; Arcas, J.; Multigner, M.; Crespo, P.; Vazquez, M.; Hernando, A.

1997-01-01

A new series of compounds Er(Fe 1-x Co x ) 11.35 Nb 0.65 were synthesized. For x≤0.4, the element Nb can stabilize the ThMn 12 -type compounds. X-ray diffraction results show that the lattice parameters a and c decrease with the substitution of Co for Fe atoms. With increasing Co content, the Curie temperature increases from T c =507 K for x=0 to T c =904 K for x=0.4. Values of the saturation magnetization at 5 K and 300 K are reported. (orig.)

Poly thiophene hydrophobic and hydrophilic compounds, silver and iodine synthesized by plasma; Compuestos hidrofobicos e hidrofilicos de politiofeno, plata y yodo sintetizados por plasma

Energy Technology Data Exchange (ETDEWEB)

Palacios, J.C.; Chavez, J.A. [IIM, UNAM, Circuito exterior, Ciudad Universitaria, 04510 Coyoacan, D.F. (Mexico); Olayo, M.G.; Cruz, G.J. [ININ, Apdo. Postal 18-1027, 11801 Mexico D.F. (Mexico)

2007-07-01

Compounds in thin films of poly thiophene with silver and poly thiophene doped with iodine and silver using splendor discharges were synthesized. It is studied the wettability of the compounds and its transport properties. It was found that the compounds can modify their hydrophilic to hydrophobic behavior controlling their surface ruggedness and the metallic content. The doped with iodine plays a fundamental paper in the modification of the ruggedness of the compounds. (Author)

Series of edge-sharing bi-triangle Ln4 clusters with a μ4-NO3- bridge: syntheses, structures, luminescence, and the SMM behavior of the Dy4 analogue.

Science.gov (United States)

Zou, Hua-Hong; Wang, Rong; Chen, Zi-Lu; Liu, Dong-Cheng; Liang, Fu-Pei

2014-02-14

A series of Ln4 clusters, [Ln4L2(μ3-OH)2(μ4-NO3)(NO3)4(OCH3)(H2O)]·xMeCN·yMeOH (Ln = Gd (1), Tb (2), Dy (3), Ho (4), Er (5), Yb (6), L = 2-{[2-(2-hydroxy-ethoxy)-ethylimino]-methyl}-6-methoxyphenol), have been synthesized by the reaction of Ln(NO)3 and a Schiff-base ligand formed in situ. The six complexes display similar structures, with an overall metal core comprising two edge-sharing triangular Ln3 units linked by a μ4-NO3(-) bridge. The luminescence spectrum of complex 2 shows the characteristic emission of the Tb(III) ions. The magnetic susceptibility studies reveal that the Ln(III) ions are very weakly interacting in all six compounds. Frequency dependence of the ac-susceptibility was found for 3, suggesting a typical single-molecule magnet (SMM) behavior with an anisotropic barrier of 28 K.

Experimental and theoretical characterization of organic salt: 2-((4-bromophenyl)amino) pyrido[1,2-a] quinoxalin-11-ium bromide monohydrate synthesized via oxidative cyclization

Science.gov (United States)

Faizi, Md. Serajul Haque; Alam, Mohammad Jane; Haque, Ashanul; Ahmad, Shabbir; Shahid, M.; Ahmad, Musheer

2018-03-01

Quinoxalines are nitrogen-embedded heterocyclic compounds that possess unique and versatile pharmacological applications. The present article describes synthesis and characterization of organic salt 2-((4-bromophenyl)amino)pyrido [1,2-a]quinoxalin-11-ium bromide (BAPQ), an oxidative cyclized product of N-phenyl-N-(pyridine-2-ylmethylene)benzene-1,4-diamine (PPMD). The structure of the synthesized product was extensively characterized by 1H NMR, 2D-COSY NMR, MS, IR, UV-vis, X-ray techniques and elemental analysis. The electronic and structural properties of BAPQ was well complemented by performing extensive computational studies (B3LYP/6-311G (d,p) basis sets). Metal-free, mild reaction condition, easy work-up and excellent yield with high purity are main features of this work and thus holds promise for the generation of new compounds of this class. Analytical results indicated ionic nature of the compound with bromide as counterion. DFT calculation showed low kinetic stability and high reactivity of the compound.

The syntheses, characterization and in vitro metabolism of nitracaine, methoxypiperamide and mephtetramine.

Science.gov (United States)

Power, John D; Scott, Kenneth R; Gardner, Elizabeth A; Curran McAteer, Bronagh M; O'Brien, John E; Brehon, Margaret; Talbot, Brian; Kavanagh, Pierce V

2014-01-01

Three legal highs; nitracaine (3-(diethylamino)-2,2-dimethylpropyl 4-nitrobenzoate), methoxypiperamide (MEOP, (4-methoxyphenyl)(4-methylpiperazin-1-yl)methanone) and mephtetramine (MTTA, 2-((methylamino)methyl)-3,4-dihydronaphthalen-1(2H)-one) appeared in 2013 as new psychoactive substances (NPS) on Internet websites selling 'research chemicals'. These compounds were synthesized and analyzed via our synthesize, analyze, and metabolize (SAM) protocol. Nitracaine was synthesized by the transesterification of methyl 4-nitrobenzoate with 3-(diethylamino)-2,2-dimethylpropan-1-ol. Methoxypiperamide was synthesized by the reaction of 4-methoxybenzoyl chloride with 1-methylpiperazine, and mephtetramine through the Mannich reaction of 1-tetralone with paraformaldehyde and methylamine hydrochloride. Each compound was characterized by nuclear magnetic resonance (NMR), gas chromatography with electron impact mass spectrometry (GC-EIMS), liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS), and high resolution electrospray ionization mass spectrometry (HR-ESI-MS). A sample of nitracaine was also test-purchased from an Internet vendor and its structure confirmed by GC-EIMS and LC-ESI-MS. Finally, the in vitro metabolism of the nitracaine, mephtetramine, and methoxypiperamide was investigated, using a human microsomal liver extract, in order to tentatively identify potential metabolites that may be encountered in the analysis of biological samples in clinical or toxicology labs. The use of our SAM protocol highlights the ability of academic research labs to quickly respond to and disseminate information about emerging NPS. Copyright © 2014 John Wiley & Sons, Ltd.

SYNTHESIS AND HEMOLYTIC PROPERTIES OF DERIVATIVES OF 4,4'-DIHYDROXYBIPHENYL – 2,2'-[BIPHENYL-4,4'- DIYLBIS(OXY]BIS[N-(METHYLAMINOALKILACETAMIDES

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S. O. Zanoza

2016-04-01

Full Text Available The purpose of this work was synthesis of 4,4’-dihydroxybiphenyl derivatives, namely 2,2’-[biphenyl-4,4’-diylbis(oxy]bis[N-(2-aminoalkylacetamide], study of their hemolytic properties and the effect of the side chain structure on hemolytic properties. 2,2’-[Biphenyl-4,4’-diylbis(oxy]diacetic acid was synthesized by alkylation of 4,4’-dihydroxybiphenyl with methylbromoacetate, followed by alkaline hydrolysis. Chloroanhydride was obtained by treatment of this acid with thionyl chloride. 2,2’-[Biphenyl-4,4’-diylbis(oxy]  bis-[N-(2-aminoalkylacetamides] were synthesized in the biphasic media (dichloromethane/ aqueous sodium carbonate. Structures of synthesized compounds were proved by mass-spectrometryand 1Н NMR. Hemolytic properties were studied using healthy donors’ erythrocytes 0(I/Rh+. The absence of hemolytic properties for obtained compounds was shown, unlike similar 4,4’-aminoalkoxybiphenyls for which a significant hemolysis was shown. Thus, replacement of the ethylene group with amide group in the side chain of 4,4’-bissubstituted biphenyls significantly reduces hemolytic properties.

Synthesis, physical and chemical properties of 2-((5-(hydroxy(phenylmethyl-4R-4H-1,2,4-triazole-3-ylthioacetic acids and its salts

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A. M. Rud

2018-02-01

Full Text Available Today’s a creation of new domestic medicines is very important problem for pharmacy and medicine. Therefore, it is relevant to synthesize new domestic biologically active compounds. It is known that a large number of new 3-thio and 4-amino derivatives on the basis of 1,2,4-triazole have recently been synthesized, among which compounds with high pharmacological activity have been found. Based on the experience of previous studies and with the aim of creating new original drugs, our goal was to synthesize 2-((5-(hydroxy(phenylmethyl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids series and to obtain salts on its basis, which have high indicators of pharmacological activity based on the literature data. The goal of the work is a targeted synthesis of potential low-toxic and highly effective compounds with a wide spectrum of pharmacological activity among 5-(hydroxy(phenylmethyl-4-R-4H-1,2,4-triazole-3-thione derivatives, confirmation of their individuality and structure, as well as the study of physical-chemical properties, for the further pharmacological screening. Materials and methods. 2-((5-(hydroxy(phenylmethyl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids were prepared by heating 5- (hydroxy(phenylmethyl-4-R-4H-1,2,4-triazol-3-thiones with chloroacetic acid. Subsequently, the synthesized thioacetic acids were subject for modification. Salts of 2-((5-(hydroxy(phenylmethyl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids were obtained by reacting thioacetic acids with equivalents of sodium or potassium hydroxides. To obtain Iron(II, Copper(II or Zinc(II salts, half-molar amounts of the appropriate sulfates were added to the obtained solutions. Salts of 2-((5-(hydroxy(phenylmethyl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids with organic bases were obtained by the reaction of acids with piperidine or morpholine in ethanol medium. Results. During the synthetic studies, 13 previously undescribed new compounds were obtained. The individuality of 2-((5-(hydroxy

Preparation and properties of organo(acetylacetonato)antimony(V) compounds

NARCIS (Netherlands)

Meinema, H.A.; Noltes, J.G.

Organo(acetylacetonato)antimony(V) compounds of the types R2SbCl2Acac, R4SbAcac, PhSbCl3Acac and Cl4SbAcac have been synthesized. The compounds are monomeric in solution. IR and PMR data of these compounds, which contain a chelated Acac ligand have been discussed. Ph2SbCl2Acac shows abnormal

Syntheses, Magnetic and Spectral Studies on the Coordination Compounds of the Polystyrene-anchored Thiazolidin-4-one

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Dinesh Kumar

2012-01-01

Full Text Available The reaction between polystyrene 3-formylsalicylate and thiophene-2-carboxylic acid hydrazide in DMF in the presence of ethyl acetate results in the formation of polystyrene N-(2-carbamoylthienyl-3'-carboxy-2'-hydroxybenzylideneimine (I. A benzene suspension of I reacts with mercaptoacetic acid and forms the polystyrene N-(2-carbamoylthienyl-C-(3'-carboxy-2'-hydroxyphenyl thiazolidin-4-one, PSCH2–LH2 (II. A DMF suspension of II reacts with Zn(II, Co(II, Cu(II, Zr(OH2(IV and MoO2(VI ions and forms the corresponding polystyrene-anchored coordination compounds, [PSCH2–LZn(DMF] (III, [PSCH2–LCo(DMF3] (IV, [PSCH2–LHCu(OAc] (V, [PSCH2–LH2Zr(OH2(OAc2] (VI and [PSCH2–LHMoO2(acac] (VII respectively. The polystyrene-anchored coordination compounds have been characterized on the basis of elemental analyses, spectral (IR, reflectance, ESR studies and magnetic susceptibility measurements. II acts as a neutral tridentate ONS donor ligand in VI, a monobasic bidentate OS donor ligand in VII, a monobasic tridentate ONS donor ligand in V and a dibasic tridentate ONO donor ligand in III and IV. The acetato groups behave as monodentate ligands in V and VI. A square-planar structure for V, a tetrahedral structure for III, an octahedral structure for IV and VII and a pentagonal-bipyramidal structure for VI are suggested.

Syntheses and characterizations of LiFePO4 powders

OpenAIRE

Jugović, Dragana; Kuzmanović, Maja; Mitrić, Miodrag; Cvjetićanin, Nikola; Uskoković, Dragan

2011-01-01

The olivine type compositions LiMPO4 (M = Fe, Mn, Co) are among the most attractive materials for the positive electrode of lithium-ion battery. The benefits of using LiFePO4 are excellent cycle life, high structural stability, low cost and environmental friendliness. Here will be presented our efforts to obtain LiFePO4 powders through several synthesis methods. The differences in phase purity, microstructure, morphology, and electrochemical performances of synthesized powders were investigat...

Investigations in anhydrous liquid ammonia. Reaction of group 2, 4, 5, 11 metal and actinoids compounds

International Nuclear Information System (INIS)

Woidy, Patrick

2014-01-01

The solubility and reactivity of metal halides, transition metal halides, and actinoid halides in liquid ammonia can lead to new starting materials for the synthesis of fluorides in low oxidation states or for nitrides via a ''low-temperature route''. In this context the ability of metal and actinoid halides to act as an acceptor for or donor of fluoride ions is also of interest. Four different systems were investigated in this study. In the first section, the synthesis and characterization of new compounds were carried out in the system CuX/NH 3 (X = F, Cl, Br, I, and CN) and lead to a ligand stabilized monovalent copper fluoride as a main result. In the second section, the solubility of uranyl compounds and uranium halides in liquid ammonia was investigated and the products were characterized. In the third section, alkali metal thorates were synthesized. Their solubility in liquid ammonia and their behavior as an acceptor for fluoride ions was investigated. In the last section, the results on the solubility behavior of transition metal halides in liquid ammonia and their coordination behavior are presented. In the first system CuX/NH 3 several new compounds, such as [Cu(NH 3 ) 3 ]X (X = Br, I or CN) were synthesized and characterized. The reactions of this compounds with fluoride ion donors (NH 4 F or Me 4 NF) led unfortunately not to the monovalent copper fluoride CuF. The comproportionation reaction of Cu and CuF 2 in liquid ammonia lead to the compounds [Cu(NH 3 ) 3 ] 2 [Cu 2 (NH 3 ) 2 ] . 4 NH 3 and [Cu(NH 3 ) 2 ]F . NH 3 . For the preparation of binary CuF, various decomposition experiments were executed on the compound [Cu(NH 3 ) 2 ]F . NH 3 which resulted in different decomposition products. In additional studies various complexes of divalent copper was investigated and with the compound [Cu(NH 3 ) 5 ]F 2 . NH 3 the solubility of fluoride containing substances in liquid ammonia could be shown. Studies of six- and tetravalent uranium

Synthesis and physical-chemical properties of 2-((4-R-3-(morpholinomethylen-4H-1,2,4-triazole-5ylthioacetic acid

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R. О. Shcherbyna

2014-12-01

Full Text Available The creation and improvement of the original domestic medicines is anactual problem of medical and pharmaceutical industries. Chemistry of heterocyclicsystems attracts scientists all over the world, as it is associated with a number of properties of this class of compounds which allow to use them for various purposes. It is known that the morpholine salts of 2-((4-R-5-R1-4H-1,2,4-triazoles-3-ylthioacetic acids exhibit low toxicity and pronounced pharmacological effect. The additional morpholine moiety in the 1,2,4-triazole’s nucleusshould lead to compounds with high biological activity. The aim of researchis the synthesis of 2-((4-R-3-(morpholinomethylen-4H-1,2,4-triazole-5-ylthioaceticacidsand determination of its physical-chemical properties. Materials and methods.The determinationof physical-chemical propertiesof the obtained compounds has been carried out according to the methods listed in the State Pharmacopoeia of Ukraine. The determinationof melting temperature has been performed for the synthesized compounds (device OptiMelt Stanford Research Systems MPA100. The structure of the compoundshas been confirmed by 1H NMR spectroscopy (Mercury 400, chromatography-mass spectrometry (Agilent 1260 Infinity device with mass detector Agilent 6120 LC / MS and elemental analysis (ElementarVario L cube. Results.14 new synthesized compounds, namely isopropyl 2-morpholinoacetate, 2-morpholinoacetohydrazide, N-R-2-(2-morpholinoacetylhydrazinecarbothioamides, 2-(2-morpholinoacetyl-hydrazinecarbothioamide, 3-(morpholinomethyl-4-R-4H-1,2,4-triazole-5-thiolesand2-((4-R-3-(morpholinomethylen-4H-1,2,4-triazole-5-ylthioaceticacid(where, R=H, CH3, C2H5,C6H5 have been studied.The fragmentation of 2-((4-ethyl-3-(morpholinomethyl-4H-1,2,4-triazol-5-ylthioacetic acid has been carried out usingmethod of LC/MS and fragment ions have been identified. The structure of the synthesized compounds in all cases has been confirmed by modern instrumental methods of analysis

Syntheses, structural analyses and luminescent property of four alkaline-earth coordination polymers

International Nuclear Information System (INIS)

Zhang, Sheng; Qu, Xiao-Ni; Xie, Gang; Wei, Qing; Chen, San-Ping

2014-01-01

Four alkaline-earth coordination polymers, [Ba(Pzdc)(H 2 O)] n (1), [Ba(Pzdc)] n (2), [AgSr(Pzdc)(NO 3 )(H 2 O)] n (3), [Ag 2 Ca(Pzdc) 2 (H 2 O)] n (4) (H 2 Pzdc=2, 3-pyrazinedicarboxylic acid) have been synthesized and characterized by single-crystal X-ray diffraction. Compounds 1 and 2 afford 2D layer networks generated by one-dimensional chains containing the [Ba 2 O 11 N] units. Compound 3 is of 2D mixed-metal coordination network formed by one-dimensional chain units, while 4 is of a 3D heterometallic framework. Interestingly, 1 and 2 can undergo reversible SCSC structural transformation upon dehydration/rehydration of coordinated water molecules. In addition, the π–π stacking interactions dominate fluorescent properties of compounds 1 and 2. - Graphical abstract: Four new coordination polymers [Ba(Pzdc)(H 2 O)] n (1), [Ba(Pzdc)] n (2), [AgSr(Pzdc)(NO 3 )(H 2 O)] n (3), [Ag 2 Ca(Pzdc) 2 (H 2 O)] n (4) (H 2 Pzdc=2, 3-pyrazinedicarboxylic acid) have been synthesized. Compounds 1–3 display 2D topology structures and compound 4 exhibits a 3D topology structure. Fortunately, 1 and 2 undergo reversible dehydration/rehydration of coordinated water molecules. Display Omitted - Highlights: • All structures are generated by 1D chains. • 1 and 2 show reversible dehydration/rehydration of coordinated water molecules. • The π–π stacking interactions dominate fluorescent properties of compounds 1 and 2

In-vitro antimicrobial screening and molecular docking studies of synthesized 2-chloro-N-(4-phenylthiazol-2-ylacetamide derivatives

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Rahmat Ali

2015-01-01

Full Text Available Introduction: Glucosamine-6-phosphate (GlcN6P synthase biosynthetic pathway has been identified as potential targets for the development of new antimicrobial agents. Aim: A series of 2-chloro-N-(42-phenylthiazol-25-ylacetamide derivatives (3a-r was synthesized and evaluated their antimicrobial activity. Materials and Methods: The 2-chloro-N-(Para substituted phenylthiazol-25-yl acetamide (2a-c were synthesized by stirring intermediates (1a-c with 2-chloroacetylchloride in dichloromethane in the presence of K2CO3. The intermediate (2a-c were further reacted with different secondary amine such as pyrrolidine, N-methyl piperazine, N-ethyl piperazine, thiomorpholine, morpholine, piperidine etc in ethanol in presence of TEA Triethylamine (TEA to get desired compounds (3a-r. Compounds were characterized by a spectroscopic technique such as Fourier transform infraredFTIR, 1 H-NMR, 13 C-NMR, and mass spectrometry. The synthesized thiazole derivatives (3a-r were screened for anti-bacterial and anti-fungal activity against Escherichia coli, Staphylococcus aureus NCTC 6571, Pseudomonas aeruginosa NCTC 10662, CandidaC. albicans (MTCC-183, AspergillusA. niger (MTCC 281 NCTC 10418 and AspergillusA. flavus (MTCC 277. Result and Conclusion: The results of anti-bacterial screening revealed that among all the screened compounds, eight compounds viz. 3b, 3c, 3d, 3e, 3i, 3j, 3k, and 3p showed moderate to good anti-bacterial and antifungal activity having minimum inhibitory concentration (MIC between 6.25- and 25 µg/ml. While compound 3d showed the most promising antibacterial activity against E. coli and S. aureus, while the compound 3j showed promising antifungal activity with MIC value 6.25 µg/ml against C. albicans, A. niger and A. flavus. In addition, all these eight potential molecules were also examined for possible binding on enzyme GlcN6Pglucosamine-6-phosphate synthase by molecular docking studies on (PDB ID 1JXA.

Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

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K. Jeyadheepan

2014-01-01

Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

SYNTHESIS AND ANTITUMOR ACTIVITY OF COPPER, NICKEL AND COBALT COORDINATION COMPOUNDS WITH 1-(2-HYDROXYPHENYL)ETHANONE N(4)-ALLYL-3-THIOSEMICARBAZONE

OpenAIRE

Vasilii GRAUR; Serghei SAVCIN; Victor TSAPKOV; Aurelian GULEA

2015-01-01

The paper presents the synthesis of the ligand 1-(2-hydroxyphenyl)ethanone N(4)-allyl-3-thiosemicarbazone (H2L) and six coordination compounds of copper, nickel and cobalt with this ligand. The structure of thiosemicarbazone H2L was studied using 1H and 13С NMR spectroscopy. The synthesized coordination compounds were studied using elemental analysis, gravimetric analysis of water content, molar conductivity, and magnetochemistry. For H2L the antitumor activity towards human leukemia HL-60 ce...

Synthesis, pharmacological evaluation and molecular docking studies of pyrimidinedione based DPP-4 inhibitors as antidiabetic agents

Science.gov (United States)

Jha, Vibhu; Bhadoriya, Kamlendra Singh

2018-04-01

Dipeptidyl peptidase-4 (DPP-4) inhibitors are a class of newly developed antidiabetic drugs that bock DPP-4. DPP-4 is responsible for degradation of incretins harmones such as GLP-1 (Glucagon like Peptide) and GIP (Gastric inhibitory polypeptide) that maintain blood-glucose level. Pyrimidinedione based compounds were designed and synthesized for DPP-4 inhibitory activity. These heterocycles were designed by taking Alogliptin as a reference DPP-4 inhibitors and synthesized as N-methylated and N-benzylated pyrimidinediones. These compounds were subjected to DPP-4 assay, five out of nine synthesized compounds have shown in vitro DPP-4 inhibitory activity in significant range. Further, molecular docking studies of these compounds were performed on DPP-4 subunit and compared with natural DPP-4 inhibitors like Flavone, Resveratrol, Quercetin, Diprotin A. Docking studies have led to the conclusion that there are some identical amino acid interactions as Tyr 666 and Tyr 662, seen in both synthesized compounds and natural DPP-4 inhibitors. This study completely gives a good scope for further derivatisation and optimization of synthesized compounds to get clinical candidate as DPP-4 inhibitor for antidiabetic activity.

Synthesis and photodegradation studies of analogues of muscle relaxant 1,4-dihydropyridine compounds

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Gündüz Miyase Gözde

2017-09-01

Full Text Available This paper describes the synthesis of 1,4-dihydropyridine compounds (DHPs endowed with good muscle relaxant activity and stability to light. Six new condensed DHPs were synthesized by the microwave irradiation method. A long-chain ester moiety [2-(methacryloyloxyethyl] and various substituents on the phenyl ring were demonstrated to affect the muscle relaxant activity occurring in isolated rabbit gastric fundus smooth muscle strips. Forced photodegradation conditions were applied to the molecules according to the ICH rules. The degradation profile of the drugs was monitored by spectrophotometry coupled with the multivariate curve resolution technique. Formation of the oxidized pyridine derivative was observed for all the studied DHPs, except for one compound, which showed very fast degradation and formation of a second photo-product. Pharmacological tests on the molecules showed a good muscle relaxing effect, with a mechanism similar to that of nifedipine, however, proving to be more stable to light.

Synthesis and Antimicrobial Evaluation of Some Novel 2-(4-Chlorophenylimino) thiazolidin-4-one Derivatives

Energy Technology Data Exchange (ETDEWEB)

B' Bhatt, H.; Sharma, S. [Hemchandracharya North Gujarat Univ., Gujarat (India)

2012-06-15

A series of 2-(4-chlorophenylimino)-5-((3-(p-substituted phenyl)-1-phenyl-1H-pyrazol-4-yl) methylene) thiazolidin-4-one (3a-h) compounds were prepared from the 2-(4-chlorophenylimino) thiazolidin-4-one (1) and 1-phenyl-3-(psubstituted phenyl)-1H-pyrazole-4-carbaldehyde (2a-h). All compounds were characterized by elemental (C, H, N) analysis and spectral (FT-IR, {sup 1}H NMR and GC-MS) analysis. These newly synthesized compounds were screened for their antibacterial and antifungal activities. Antimicrobial activity was observed and evaluated against the bacterial strains like Eschericha coli (MTCC 443), Pseudomonas aeruginosa (MTCC 1688), Staphylococcus aureus (MTCC 96), Streptococcus pyogenes (MTCC 442) and against the fungal strains like Candida albicans (MTCC 227), Aspergillus niger (MTCC 282) and Aspergillus clavatus (MTCC 1323). All the synthesized compounds were found to possess moderate to excellent antimicrobial activity against above selected strains.

Synthesis, physical and chemical properties of 2-((4-(R-amino-5-(thiophen-2-ylmethyl-4H-1,2,4-triazol-3-ylthioacetic acids salts

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А.А. Safonov

2017-12-01

Full Text Available Thanks to the rapid development of science, humanity has achieved remarkable success in various fields. This also applies to the synthesis of biological compounds. Over the centuries, scientists have invented many methods and drugs that are being actively used to date. Derivatives of 1,2,4-triazole can be the foundation for the manufacture of new native drugs that will compete with foreign ones. The aim of work was synthesis and confirmation the structure of 2-((4-(R-amino-5-(thiophen-2-ylmethyl-4H-1,2,4-triazol-3-ylthioacetate acids salts. Materials and methods. As starting substances we used 2-((4-(R-amino-5-(thiophen-2-ylmethyl-4H-1,2,4-triazol-3-ylthioacetic acids, which were synthesized by previously described methods. The structure of synthesized compounds was confirmed by the complex use of modern physical-chemical methods of analysis: elemental analysis, 1H-NMR spectroscopy, HPLC-MS. Results. Salts of 2-((4-(R-amino-5-(thiophen-2-ylmethyl-4H-1,2,4-triazol-3-ylthioacetic acids were synthesized by the interaction of the appropriate acids with organic (morpholin, methanamin, 2-hydroxyethanamin, inorganic basics (aqueous ammonia solution, sodium hydroxide and salts (zinc sulfate, ferrum (III chloride, magnesium sulfate, copper (II sulfate in alcoholic or aqueous media. Conclusions. A series of novel 2-((4-(R-amino-5-(thiophen-2-ylmethyl-4H-1,2,4-triazol-3-ylthioacetic acids salts were synthesized. The structure of synthesized compounds is established using modern physical-chemical methods of analysis.

Synthesis and pharmacological investigation of 2-(4-dimethylaminophenyl)-3,5-disubstituted thiazolidin-4-ones as anticonvulsants.

Science.gov (United States)

Senthilraja, Manavalan; Alagarsamy, Veerachamy

2012-10-01

A new series of 2-(4-dimethylaminophenyl)-3-substituted thiazolidin-4-one-5-yl-acetyl acetamides/benzamides were synthesized by the nucleophilic substitution of 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetylchloride with acetamide and benzamide. The starting material 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetylchloride was synthesized from 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetic acid, which in turn was prepared by one-pot reaction of amino component, p-dimethylamino benzaldehyde and mercapto succinic acid. The title compounds were investigated for their anticonvulsant activities; among the test compounds, compound 2-(4-dimethylaminophenyl)-3-phenylamino-thiazolidine-4-one-5-yl-acetylbenzamide (14) emerged as the most active compound of the series and as moderately more potent than the reference standard diazepam. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Syntheses, structural analyses and luminescent property of four alkaline-earth coordination polymers

Energy Technology Data Exchange (ETDEWEB)

Zhang, Sheng; Qu, Xiao-Ni; Xie, Gang; Wei, Qing; Chen, San-Ping, E-mail: sanpingchen@126.com

2014-02-15

Four alkaline-earth coordination polymers, [Ba(Pzdc)(H{sub 2}O)]{sub n} (1), [Ba(Pzdc)]{sub n} (2), [AgSr(Pzdc)(NO{sub 3})(H{sub 2}O)]{sub n} (3), [Ag{sub 2}Ca(Pzdc){sub 2}(H{sub 2}O)]{sub n} (4) (H{sub 2}Pzdc=2, 3-pyrazinedicarboxylic acid) have been synthesized and characterized by single-crystal X-ray diffraction. Compounds 1 and 2 afford 2D layer networks generated by one-dimensional chains containing the [Ba{sub 2}O{sub 11}N] units. Compound 3 is of 2D mixed-metal coordination network formed by one-dimensional chain units, while 4 is of a 3D heterometallic framework. Interestingly, 1 and 2 can undergo reversible SCSC structural transformation upon dehydration/rehydration of coordinated water molecules. In addition, the π–π stacking interactions dominate fluorescent properties of compounds 1 and 2. - Graphical abstract: Four new coordination polymers [Ba(Pzdc)(H{sub 2}O)]{sub n} (1), [Ba(Pzdc)]{sub n} (2), [AgSr(Pzdc)(NO{sub 3})(H{sub 2}O)]{sub n} (3), [Ag{sub 2}Ca(Pzdc){sub 2}(H{sub 2}O)]{sub n} (4) (H{sub 2}Pzdc=2, 3-pyrazinedicarboxylic acid) have been synthesized. Compounds 1–3 display 2D topology structures and compound 4 exhibits a 3D topology structure. Fortunately, 1 and 2 undergo reversible dehydration/rehydration of coordinated water molecules. Display Omitted - Highlights: • All structures are generated by 1D chains. • 1 and 2 show reversible dehydration/rehydration of coordinated water molecules. • The π–π stacking interactions dominate fluorescent properties of compounds 1 and 2.

Functionalized 3-(benzofuran-2-yl-5-(4-methoxyphenyl-4,5-dihydro-1H-pyrazole scaffolds: A new class of antimicrobials and antioxidants

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Javarappa Rangaswamy

2017-05-01

Full Text Available A new class of functionalized 3-(benzofuran-2-yl-5-(4-methoxyphenyl-4,5-dihydro-1H-pyrazole scaffolds (4a–q was synthesized by a four step reaction in good yields. Initially, o-alkyl derivative of salicyaldehyde (1 readily furnished corresponding 2-acetyl benzofuran (2 on treatment with potassium tert-butoxide (t-BuOK in the presence of molecular sieves. Further, Claisen–Schmidt condensation reaction with 4-methoxy benzaldehyde and hydrazine hydrate followed by coupling of benzoyl chlorides afforded target compounds (4a–q. Representative of the synthesized compounds was characterized by IR, 1H NMR, 13C NMR, mass, elemental analysis and evaluated for antimicrobial and antioxidant activities. The results gathered are allowed to conclude that, all newly synthesized analogues exhibit a certain degree of antimicrobial and antioxidant activities. Among the analogues, compounds (4h and (4j showed an excellent antimicrobial activity in the well plate method. Meanwhile, compounds (4e–f, (4l and (4p showed good antioxidant activity, whereas compound (4g and (4q displayed dominant antioxidant efficacy compared to standard butylated hydroxy anisole (BHA.

Synthesis of some biologically active 2,4’-bipyridine-5-carbonitriles carrying the 4-hydroxyphenylthio moiety

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T. KARABASANAGOUDA

2009-07-01

Full Text Available A series of new 4-aryl-2’-[(4-hydroxyphenylthio]-6oxo-1,6-dihydro-2,4’-bipyridine-5-carbonitriles (3a–k and 6-amino-4aryl-2’-[(4-hydroxyphenylthio]-2,4’-bipyridine-5-carbonitriles (4a–h were synthesized from 4-hydroxythiophenol (1. The reaction of 4-hydroxythiophenol with 4-acetyl-2-chloropyridine yielded 1-{2-[(4-hydroxyphenylthio]pyridin-4-yl}ethanone (2. Further treatment of 2 with ethyl cyanoacetate in the presence of ammonium acetate with various aromatic aldehydes furnished the compounds 3a–k. On the other hand, condensation of 2 with aromatic aldehydes in the presence of alcoholic malononitrile in ammonium acetate gave compounds 4a–h. The structures of the newly synthesized compounds were established on the basis of their elemental analysis, as well as their IR, 1H- and 13C-NMR and mass spectral data. All the title compounds were subjected to in vitro antibacterial testing against two strains and antifungal screening against two fungi. Some of the compounds showed promising activity.

Synthesis and antimicrobial activities of novel 1,4-benzothiazine derivatives

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Vijay V. Dabholkar

2016-09-01

Full Text Available A series of 2H,4H-2-[3,5-dimethyl-4-(substituted phenyl azo pyrazol-1-yl] carbonyl methyl-3-oxo-1,4-benzothiazine derivatives have been synthesized by the reaction of 2H,4H-2-hydrazino carbonyl methyl-3-oxo-1,4-benzothiazine with acetyl acetone derivatives using ultrasound in lesser time with higher yields. All the synthesized compounds were investigated for their antibacterial activities. The result indicated that the compounds show convincing activities against Gram-positive bacteria (Bacillus subtilis and Streptococcus lactis when compared with standard drug (ampicillin trihydrate. These compounds were also synthesized by conventional method and their structures have been elucidated on the basis of spectral analyses and chemical reactions.

Three new chalcohalides, Ba4Ge2PbS8Br2, Ba4Ge2PbSe8Br2 and Ba4Ge2SnS8Br2: Syntheses, crystal structures, band gaps, and electronic structures

International Nuclear Information System (INIS)

Lin, Zuohong; Feng, Kai; Tu, Heng; Kang, Lei; Lin, Zheshuai; Yao, Jiyong; Wu, Yicheng

2014-01-01

Highlights: • Three new chalcohalides: Ba 4 Ge 2 PbS 8 Br 2 , Ba 4 Ge 2 PbSe 8 Br 2 and Ba 4 Ge 2 SnS 8 Br 2 have been synthesized. • The MQ 5 Br octahedra and GeQ 4 tetrahedra form a three-dimensional framework with Ba 2+ in the channels. • Band Gaps and electronic structures of the three compounds were studied. - Abstract: Single crystals of three new chalcohalides: Ba 4 Ge 2 PbS 8 Br 2 , Ba 4 Ge 2 PbSe 8 Br 2 and Ba 4 Ge 2 SnS 8 Br 2 have been synthesized for the first time. These isostructural compounds crystallize in the orthorhombic space group Pnma. In the structure, the tetra-valent Ge atom is tetrahedrally coordinated with four Q (Q = S, Se) atoms, while the bi-valent M atom (M = Pb, Sn) is coordinated with an obviously distorted octahedron of five Q (Q = S, Se) atoms and one Br atom, showing the stereochemical activity of the ns 2 lone pair electron. The MQ 5 Br (M = Sn, Pb; Q = S, Se) distorted octahedra and the GeQ 4 (Q = S, Se) tetrahedra are connected to each other to form a three-dimensional framework with channels occupied by Ba 2+ cations. Based on UV–vis–NIR spectroscopy measurements and the electronic structure calculations, Ba 4 Ge 2 PbS 8 Br 2 , Ba 4 Ge 2 PbSe 8 Br 2 and Ba 4 Ge 2 SnS 8 Br 2 have indirect band gaps of 2.054, 1.952, and 2.066 eV respectively, which are mainly determined by the orbitals from the Ge, M and Q atoms (M = Pb, Sn; Q = S, Se)

Synthesis of Chlorinated Tetracyclic Compounds and Testing for Their Potential Antidepressant Effect in Mice

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Usama Karama

2016-01-01

Full Text Available The synthesis of the tetracyclic compounds 1-(4,5-dichloro-9,10-dihydro-9,10-ethanoanthracen-11-yl-N-methylmethanamine (5 and 1-(1,8-dichloro-9,10-dihydro-9,10-ethanoanthracen-11-yl-N-methylmethanamine (6 as a homologue of the anxiolytic and antidepressant drugs benzoctamine and maprotiline were described. The key intermediate aldehydes (3 and (4 were successfully synthesized via a [4 + 2] cycloaddition between acrolein and 1,8-dichloroanthracene. The synthesized compounds were investigated for antidepressant activity using the forced swimming test. Compounds (5, (6 and (3 showed significant reduction in the mice immobility indicating significant antidepressant effects. These compounds significantly reduced the immobility times at a dose 80 mg/kg by 84.0%, 86.7% and 71.1% respectively.

InTaO4-based nanostructures synthesized by reactive pulsed laser ablation

International Nuclear Information System (INIS)

Yoshida, Takehito; Toyoyama, Hirokazu; Umezu, Ikurou; Sugimura, Akira

2008-01-01

Nanostructured Ni-doped indium-tantalum-oxides (InTaO 4 ) were synthesized by a reactive pulsed laser ablation process, aiming at the final goal of direct splitting of water under visible sunbeam irradiation. The third harmonics beam of a Nd:YAG laser was focused onto a sintered In 0.9 Ni 0.1 TaO 4-δ target in pure oxygen background gases (0.05-1.00 Torr). Increasing the oxygen gas pressure, via thin films having nanometer-sized strong morphologies, single-crystalline nanoparticles were synthesized in the reactive vapor phases. The nanostructured deposited materials have the monoclinic layered wolframite-type structure of bulk InTaO 4 , without oxygen deficiency. (orig.)

Synthesis and enzyme inhibitory studies of some new N-alkylated/aralkylated N-(4-ethoxyphenyl)-2,3-drobenzo-(1,4)-dioxin-6-sulfonamides

International Nuclear Information System (INIS)

Abbasi, M.A.; Islam, M.; Rehman, A.U.; Siddiqui, S.Z.

2016-01-01

The research endeavor was aimed to synthesize N-alkyl/aralkylated-N-(4-ethoxyphenyl)-2,3-dihydrobenzo-(1,4)-dioxine-6 sulfonamides and to evaluate their enzyme inhibitory potential. The target molecules were synthesized in two steps. The first step involved the reaction of 4-ethoxyaniline (1) with N-2,3-dihydrobenzo(1,4)-dioxin-6-sulfonyl chloride (2) under dynamic pH control maintained by 10% aqueous Na/sub 2/CO/sub 3/ to yield N-(4-ethoxyphenyl)-2,3-dihydrobenzo-(1,4)-dioxine-6-sulfonamide (3). In second step parent compound 3 was reacted with various alkyl/aralkyl halides (4a-l) in N,N'-dimethylformamide and catalytic amount of lithium hydride to accomplish some new N-alkyl/aralkylated-N-(4-ethoxyphenyl)-2,3-dihydrobenzo-(1,4)-dioxine-6 sulfonamides (5a-l). Probable structures of the synthesized compounds were characterized by contemporary spectral techniques i.e. IR, 1H-NMR and EIMS and were finally evaluated for enzyme inhibitory potential against a-glucosidase and urease. The synthesized compounds exhibited moderate to weak therapeutic potential throughout the series. (author)

Syntheses, structures and properties of two new coordination polymers based on D-camphoric acid and 2-phenyl-4,6-diamino-1,3,5-triazine

Energy Technology Data Exchange (ETDEWEB)

Lun, Huijie; Yang, Jinghe; Jin, Linyu; Cui, Sasa; Bai, Yanlong [Henan Key Laboratory of Polyoxometalate, Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China); Zhang, Xudong [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Li, Yamin, E-mail: liyamin@henu.edu.cn [Henan Key Laboratory of Polyoxometalate, Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China)

2015-05-15

By hydrothermal method, two new coordination polymers [Co(ca)(phdat)]{sub n} (1), [Ni(ca)(phdat).0.125H{sub 2}O]{sub n} (2) (H{sub 2}ca=D-camphoric acid, phdat=2-phenyl-4,6-diamino-1,3,5-triazine) have been achieved and structurally characterized by IR, elemental analyses, X-ray single-crystal diffraction and TGA. The X-ray single-crystal diffraction reveals that compounds 1 and 2 are isostructural, both of which exhibit two-dimensional layered network built up from paddle-wheel Co{sub 2}(CO{sub 2}){sub 4}/Ni{sub 2}(CO{sub 2}){sub 4} SBUs by ca{sup 2−} ligand. In the existence of π…π stacking interactions between triazine rings and phenyl rings, the 3D networks are constructed with the hanging phdat filled between the neighboring layers. Furthermore, compounds 1–2 exhibit antiferromagnetic behavior and compound 2 displays a good activity for methanol oxidation. - Graphical abstract: Two new coordination compounds 1–2 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses, magnetic and electrochemical measurement. - Highlights: • This paper reports two new coordination polymers based on D-camphoric acid. • Both the compounds feather two-dimensional layered networks built up from paddle-wheel SBUs. • The magnetism and electrochemical property are investigated.

Coordination compounds of thorium(4) containing tris(dimethylamino)-phosphinoxide

International Nuclear Information System (INIS)

Skopenko, V.V.; Klunnik, L.A.

1983-01-01

Compounds including tris(dimethylamino)-phosphinoxide of the following composition: [ThX 4 (HMPA) 4 ] and [ThX 2 (HMPA) 4 ](BPh 4 ) 2 , where X=NCSe, N(CN) 2 =, C(CN) 3 , ONC(CN) 2 -, [C(CN) 2 C(O)NH 2 ], BPh 4 =[B(C 6 H 5 ) 4 ] - , and HMPA=OP[N(CN 3 ) 2 ] 3 are prepared by interactions of thoriUm chloride with different pseudohalogenides and sodium tetraphenylborate. Some properties of the above compoUnds are studied. Using the IR spectroscopy, the way of coordinating these compounds is determined; the X-ray crystal analysis has determined isostrUcture of compounds: [Th(NCX) 4 (HMPA) 4 ] and [ThX 2 (HMPA) 4 ](BPh 4 ) 2 , where X is Se, S

Photocatalytic Degradation of 4-Nitrophenol by C, N-TiO2: Degradation Efficiency vs. Embryonic Toxicity of the Resulting Compounds

Science.gov (United States)

Osin, Oluwatomiwa A.; Yu, Tianyu; Cai, Xiaoming; Jiang, Yue; Peng, Guotao; Cheng, Xiaomei; Li, Ruibin; Qin, Yao; Lin, Sijie

2018-06-01

The photocatalytic activity of TiO2 based photocatalysts can be improved by structural modification and elemental doping. In this study, through rational design, one type of carbon and nitrogen co-doped TiO2 (C, N-TiO2) photocatalyst with mesoporous structure was synthesized with improved photocatalytic activity in degrading 4-nitrophenol under simulated sunlight irradiation. The photocatalytic degradation efficiency of the C, N-TiO2 was much higher than the anatase TiO2 (A-TiO2) based on absorbance and HPLC analyses. Moreover, using zebrafish embryos, we showed that the intermediate degradation compounds generated by photocatalytic degradation of 4-nitrophenol had higher toxicity than the parent compound. A repeated degradation process was necessary to render complete degradation and non-toxicity to the zebrafish embryos. Our results demonstrated the importance of evaluating the photocatalytic degradation efficiency in conjunction with the toxicity assessment of the degradation compounds.

Synthesis and physical-chemical properties of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R-2,4-dihydro-3H-1,2,4-triazoles

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T. M. Kaplaushenko

2016-06-01

Full Text Available The major social and economic problem of pharmaceutical industry is the search for biologically active substances, which may become the basis of new drugs, competitive with expensive imported drugs. Analysis of literature shows that in recent decades the attention is paid to researches of heterocyclic systems as potential biologically active agents of both domestic and foreign scientists. Particular interest in this regard cause 3-thio derivatives of 1,2,4-triazoles. Despite high number of publications relating to synthesis and biological properties of 1,2,4-triazole derivatives, the structure and physical-chemical properties of these compounds are studied insufficiently. In this regard, the study of synthetic, physical-chemical and biological properties of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R1-2,4-dihydro-3H-1,2,4-triazoles in our point of view is a new, theoretically and practically significant direction. Purpose - targeted synthesis of new low-toxic and highly effective compounds with potential pharmacological activity in a series of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R-2,4-dihydro-3H-1,2,4-triazoles and the study of physical and chemical properties of the synthesized compounds. Materials and methods. As starting compounds 5-(quinoline-2-il- 2-hydroxyquinoline-4-yl-4-R1-3-thio-1,2,4-triazoles have been used. Through further cooperation with halogen alkanes (ethyl bromide, propyl bromide, amyl bromide, octyl bromide, nonyl bromide, decyl bromide, cyclohexyl chloride, benzyl chloride 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R1-2,4-dyhidro-3H-1,2,4-triazoles have been obtained. Results. 15 New compounds have been received as a result of synthetic transformations, the structure of synthesized compounds has been confirmed by modern complex of physical and chemical methods of analysis (IR-spectrophotometry, 1H NMR-spectroscopy, elemental analysis, and their individuality has been proved by

New hydride compounds of 1,4-diazabicyclo[2.2.2]octane and its dication with borine and tetrahydridoborate anion and products of their transformations

International Nuclear Information System (INIS)

Shevchenko, Yu.N.; Yashina, N.I.; Markova, O.Z.; Trachevskij, V.V.

1996-01-01

New compounds [dabcoH 2 ](BH 4 ) 2 , dabco(BH 3 ) 2 2H 2 , [dabco(BH 3 ) 2 H 2 ] n have been synthesized by means of interaction between dihydrochloride of 1,4-diazobicyclo[2.2.2] octane (dabco) and NaBH 4 in the medium of nonaqueous solvents (glyme, diglyme, tetrahydrofuran, dimethylsulfoxide) and identified by the methods of element analysis, conductometry, 1 H, 11 B, 14 N NMR, IR spectroscopy and thermal analysis. A mechanism is suggested and the conditions are defined for mutual transformations of the compounds studied. Their ability to bind reversibly molecular hydrogen has been revealed for the first time. 19 refs.; 3 figs.; 1 tab

Induction heating studies of combustion synthesized MgFe2O4 nanoparticles for hyperthermia applications

International Nuclear Information System (INIS)

Khot, V.M.; Salunkhe, A.B.; Thorat, N.D.; Phadatare, M.R.; Pawar, S.H.

2013-01-01

The structural, magnetic and ac magnetically induced heating characteristics of combustion synthesized MgFe 2 O 4 nanoparticles have been investigated for application in magnetic particle hyperthermia. As prepared nanoparticles showed ferrimagnetic behavior at room temperature with magnetization of about 33.83 emu/g at ±15 kOe. The solid state MgFe 2 O 4 nanoparticles exhibited specific absorption rate (SAR) of about 297 W/g at physiological safe range of frequency and amplitude. The increase in SAR and heating temperature in ac magnetic field was thought to be due to enhancement in magnetic hysteresis loss caused by dipole–dipole interactions in combustion synthesized MgFe 2 O 4 nanoparticles. - Highlights: ► Highly crystalline pure MgFe 2 O 4 nanoparticles were synthesized by low temperature combustion. ► Effect of ac magnetic field and nanoparticles concentration on heating characteristics of MgFe 2 O 4 nanoparticles was studied. ► Combustion synthesized MgFe 2 O 4 nanoparticles show highest specific absorption rate of 297 Wg −1 . ► The reported high value of specific absorption rate is advantageous for its use in magnetic particle hyperthermia

Synthesis, biological activity and computational studies of novel azo-compounds

International Nuclear Information System (INIS)

Ashraf, J.; Murtaza, S.; Mughal, E.U.; Sadiq, A.

2017-01-01

In the present protocol, we report the synthesis and characterization of some novel azo-compounds starting from 4-methoxyaniline and 4-aminophenazone, which were diazotized at low temperature. 4-nitrophenol, 2-aminobenzoic acid, benzamide, 4-aminobenzoic acid, resorcinol, o-bromonitrobenzene and 2-nitroaniline were used as active aromatic coupling compounds for the second step. The synthesized compounds were investigated for their potential antibacterial activities by using disc diffusion method against Escherichia coli, Shigellasonnei, Streptococcus pyrogenes, Staphylococcus aureus and Neisseria gonorrhoeae strains. They were also subjected to antioxidant activities by using DPPH method. Results revealed that the compounds of 4-methoxyaniline and 4-aminophenazone showed good antibacterial activity against all strains, where as some azo-compounds have moderate to good antioxidant activities. Furthermore, these compounds were studied by computational analysis. (author)

A new three-dimensional cobalt phosphate: Co 5(OH 2) 4(HPO 4) 2(PO 4) 2

Science.gov (United States)

Han, Zhangang; Tian, Aixiang; Peng, Jun; Zhai, Xueliang

2006-10-01

A three-dimensional (3D) cobalt phosphate: Co 5(OH 2) 4(HPO 4) 2(PO 4) 2 ( 1), has been synthesized by hydrothermal reaction and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic techniques. The title compound is a template free cobalt phosphate. Compound 1 exhibits a complex net architecture based on edge- and corner-sharing of CoO 6 and PO 4 polyhedra. The magnetic susceptibility measurements indicated that the title compound obeys Curie-Weiss behavior down to a temperature of 17 K at which an antiferromagnetic phase transition occurs.

1-(4-(6-Fluorobenzo [d] isoxazol-3-yl) piperidin-1-yl)-2-(4-(hydroxymethyl)-1H-1,2,3-triazol-1-yl) ethanone: Synthesis, spectroscopic characterization, Hirshfeld surface analysis, cytotoxic studies and docking studies

Science.gov (United States)

Govindhan, M.; Viswanathan, V.; Karthikeyan, S.; Subramanian, K.; Velmurugan, D.

2017-08-01

Compound 1-(4-(6-fluorobenzo[d] isoxazol-3-yl) piperidin-1-yl)-2-(4-(hydroxymethyl)-1H-1, 2,3-triazol-1-yl) ethanone was synthesized in good yield by using click chemistry approach with 2-azido-1-(4-(6-flurobenzo[d]isooxazol-3-yl)piperidin-1-yl)ethanone as a starting material. The synthesized compound was characterized using IR, NMR and MS studies. Thermal stability of the compound was analyzed by using TGA and DSC technique. The single crystal XRD analysis was taken part, to confirm the structure of the compound. The intercontacts in the crystal structure are analyzed using Hirshfeld surfaces computational method. Cytotoxicity of the synthesized compound was evaluated and the results were reported. The binding analysis carried out between the newly synthesized molecule with human serum albumin using fluorescence spectroscopy technique to understand the pharmacokinetics nature of the compound for further biological application. The molecular docking studies were evaluated for the compound to elucidate insights of new molecules in carrier protein.

Titanium zirconium and hafnium coordination compounds with vanillin thiosemicarbazone

International Nuclear Information System (INIS)

Konunova, Ts.B.; Kudritskaya, S.A.

1987-01-01

Coordination compounds of titanium zirconium and hafnium tetrachlorides with vanillin thiosemicarbazone of MCl 4 x nLig composition, where n=1.5, 4 for titanium and 1, 2, 4 for zirconium and hafnium, are synthesized. Molar conductivity of ethanol solutions is measured; IR spectroscopic and thermochemical investigation are carried out. The supposition about ligand coordination via sulfur and azomethine nitrogen atoms is made. In all cases hafnium forms stable compounds than zirconium

Synthesis of Schiff and Mannich Bases of Isatin Derivatives with 4-Amino-4,5-Dihydro-1H-1,2,4-Triazole-5-Ones

Directory of Open Access Journals (Sweden)

Hakan Bektas

2008-09-01

Full Text Available Ethyl imidate hydrochlorides 1 were prepared by passing HCl gas through solutions of substituted benzyl cyanides and absolute ethanol. Ethoxycarbonylhydrazones 2 were synthesized from the reaction of compounds 1 with ethyl carbazate. Treatment of 2 with hydrazine hydrate leads to the formation of substituted 4-amino-4,5-dihydro-1H-1,2,4-triazole-5-ones 3. Isatin and 5-chloroisatin were added to 3 to form Schiff bases 4 and N-Mannich bases 5 of these compounds were synthesized by reacting with formaldehyde and piperidine. Their chemical structures were confirmed by means of IR, 1H- and 13C-NMR data and by elemental analysis.

Special syntheses of certain organic iodine compounds

International Nuclear Information System (INIS)

Henry, R.; Debuchy, D.; Junod, E.

1960-01-01

The technical difficulties encountered in working on radioactive products force us to choose the simplest methods of chemical synthesis possible. For iodine compounds, two special methods have been chosen: - by using fission recoil, we can prepare simple iodine compounds such as iodobenzene or methyl iodide in high yields and having a good degree of purity. The method consists in the irradiation of mixtures of uranium oxide and benzoic acid or ammonium acetate. The iodised product is separated by distillation, after dissolving the recoil medium in a solvent. - by isotopic exchange between the inorganic iodine of different valencies and complex molecules such as Bengal pink, and diodone, it is also possible to obtain satisfactory labelling yields. These reactions have been adapted so as to give a minimum time for isotopic exchange. In the case of Bengal pink, we have found a yield of 90 per cent after 60 minutes by exchange between Nal and the organic molecule in aqueous solution in presence of hydrogen peroxide. For diodone the method proposed by Liebster has been modified so as to reduce losses during purification. The analytical methods adopted for these different compounds are described. (author) [fr

[3+2] Cycloadditions of 1-halo-1-nitroethenes with (Z-C-(3,4,5-trimethoxyphenyl-N-methyl-nitrone as regio- and stereocontrolled source of novel bioactive compounds: preliminary studies

Directory of Open Access Journals (Sweden)

Radomir Jasiński

2016-07-01

Full Text Available Preliminary experiments shows, that [3+2] cycloadditions reactions proceeds with full regioselectivity and high stereoselectivity. In consequence, 3,4-trans-2-methyl-3-(3,4,5-trimethoxyphenyl-4-halo-4-nitroisoxazolidines are forming as predominantly (or sole products. Additionally, prognosis for the synthesized compounds to be potential ingredients of drugs is good.

Discovery Strategies of Bioactive Compounds Synthesized by Nonribosomal Peptide Synthetases and Type-I Polyketide Synthases Derived from Marine Microbiomes

Science.gov (United States)

Amoutzias, Grigoris D.; Chaliotis, Anargyros; Mossialos, Dimitris

2016-01-01

Considering that 70% of our planet’s surface is covered by oceans, it is likely that undiscovered biodiversity is still enormous. A large portion of marine biodiversity consists of microbiomes. They are very attractive targets of bioprospecting because they are able to produce a vast repertoire of secondary metabolites in order to adapt in diverse environments. In many cases secondary metabolites of pharmaceutical and biotechnological interest such as nonribosomal peptides (NRPs) and polyketides (PKs) are synthesized by multimodular enzymes named nonribosomal peptide synthetases (NRPSes) and type-I polyketide synthases (PKSes-I), respectively. Novel findings regarding the mechanisms underlying NRPS and PKS evolution demonstrate how microorganisms could leverage their metabolic potential. Moreover, these findings could facilitate synthetic biology approaches leading to novel bioactive compounds. Ongoing advances in bioinformatics and next-generation sequencing (NGS) technologies are driving the discovery of NRPs and PKs derived from marine microbiomes mainly through two strategies: genome-mining and metagenomics. Microbial genomes are now sequenced at an unprecedented rate and this vast quantity of biological information can be analyzed through genome mining in order to identify gene clusters encoding NRPSes and PKSes of interest. On the other hand, metagenomics is a fast-growing research field which directly studies microbial genomes and their products present in marine environments using culture-independent approaches. The aim of this review is to examine recent developments regarding discovery strategies of bioactive compounds synthesized by NRPS and type-I PKS derived from marine microbiomes and to highlight the vast diversity of NRPSes and PKSes present in marine environments by giving examples of recently discovered bioactive compounds. PMID:27092515

Discovery Strategies of Bioactive Compounds Synthesized by Nonribosomal Peptide Synthetases and Type-I Polyketide Synthases Derived from Marine Microbiomes

Directory of Open Access Journals (Sweden)

Grigoris D. Amoutzias

2016-04-01

Full Text Available Considering that 70% of our planet’s surface is covered by oceans, it is likely that undiscovered biodiversity is still enormous. A large portion of marine biodiversity consists of microbiomes. They are very attractive targets of bioprospecting because they are able to produce a vast repertoire of secondary metabolites in order to adapt in diverse environments. In many cases secondary metabolites of pharmaceutical and biotechnological interest such as nonribosomal peptides (NRPs and polyketides (PKs are synthesized by multimodular enzymes named nonribosomal peptide synthetases (NRPSes and type-I polyketide synthases (PKSes-I, respectively. Novel findings regarding the mechanisms underlying NRPS and PKS evolution demonstrate how microorganisms could leverage their metabolic potential. Moreover, these findings could facilitate synthetic biology approaches leading to novel bioactive compounds. Ongoing advances in bioinformatics and next-generation sequencing (NGS technologies are driving the discovery of NRPs and PKs derived from marine microbiomes mainly through two strategies: genome-mining and metagenomics. Microbial genomes are now sequenced at an unprecedented rate and this vast quantity of biological information can be analyzed through genome mining in order to identify gene clusters encoding NRPSes and PKSes of interest. On the other hand, metagenomics is a fast-growing research field which directly studies microbial genomes and their products present in marine environments using culture-independent approaches. The aim of this review is to examine recent developments regarding discovery strategies of bioactive compounds synthesized by NRPS and type-I PKS derived from marine microbiomes and to highlight the vast diversity of NRPSes and PKSes present in marine environments by giving examples of recently discovered bioactive compounds.

Syntheses and absorption-structure relationships of some new ...

Indian Academy of Sciences (India)

New biheterocyclic compound was synthesized as starting material to prepare new photosensitizers mono-, tri-, substituted tri-, azadimethine and mixed cyanine dyes. Absorption-structure relationship of the synthesized cyanine dyes were determined by studying their electronic spectral behaviour in ethanol. The structure of ...

Three PbII coordination polymers based on 2-(pyridin-2-yl)-1H-imidazole-4,5-dicarboxylic acid: Syntheses, crystal structures, and fluorescent properties

International Nuclear Information System (INIS)

Yu, Xiao-Yang; Xin, Rui; Gao, Wei-Ping; Wang, Na; Zhang, Xiao; Yang, Yan-Yan; Qu, Xiao-Shu

2013-01-01

Three lead coordination polymers, [PbCl(C 10 H 6 N 3 O 4 )(H 2 O)·H 2 O] n (1), [Pb(C 10 H 6 N 3 O 4 ) 2 (H 2 O)] n (2) and [Pb 3 (C 10 H 5 N 3 O 4 ) 3 ] n (3) (C 10 H 7 N 3 O 4 =2-(pyridin-2-yl)-1H-imidazole-4,5-dicarboxylic acid), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. In 1, Cl anions connected neighboring wave-like 2D layers, which are constructed with left- and right-handed helical chains, into a 3D network structure with a (6 3 )(6 5 ·8) topology. In 2, Pb cations are linked into a 3D 6 6 network with left- and right-handed helixes by μ 2 -bridging C 10 H 6 N 3 O 4 − ligands. In 3, C 10 H 5 N 3 O 4 2− ligands link Pb 6 O 12 clusters into a 3D (4 12 ·6 3 ) network. Their fluorescent properties were also investigated. - Graphical abstract: Three 3D lead compounds based on 2-(pyridin-2-yl)-1H-imidazole-4,5-dicarboxylic acid have been hydrothermally synthesized. Four new coordination modes of the organic ligand are first reported. Display Omitted - Highlights: • Three new Pb(II) complexes have been synthesized and characterized. • Left- and right-handed helical chains can be found in the 3D networks of 1 and 2. • Pb 6 O 12 clusters are connected into (4 12 ·6 3 ) network in 3

Magnetic response of polycrystalline YBaCo4O7+δ synthesized through the physical and chemical route: The role of phase inhomogeneities

International Nuclear Information System (INIS)

Vallejos, E.; Galeano, V.; Gómez, L.; Izquierdo, J.L.; Montoya, J.F.; Mera, J.; Córdoba, C.; Gómez, A.; Paucar, C.; Morán, O.

2014-01-01

Polycrystalline YBaCo 4 O 7+δ samples were obtained through a standard solid state reaction, and their structural, morphological, electrical, and magnetic properties are carefully studied. The X-ray powder diffraction (XRD) patterns showed reflections of a pure hexagonal structure (space group P6 3 mc) with lattice parameters being very close to those reported in the literature. Although XRD analysis showed that the main phase present is 114, the presence of secondary phases could not be ruled out based solely on the XRD characterization. Indeed, sensitive SQUID magnetic measurements showed that the samples were affected by very small quantities of the 112 phase (YBaCo 2 O 5.5 ), which typically manifests itself through a conspicuous increase in the magnetization at∼300 K. The results achieved corroborated the predictions concerning the difficulty of stabilizing the 114 phase when synthesized via the standard solid-state reaction. With this in mind, we next attempted to obtain the compound with improved phase purity. In so doing, the YBaCo 4 O 7+δ compound was synthesized through a wet chemistry method based on a citrates route. The XRD patterns recorded for these samples revealed well-defined peaks corresponding to a pure hexagonal structure. More interestingly, SQUID measurements show no sign of features in the M(T) curve at temperatures as low as∼80 K. This result was consistent with the magnetic behavior observed in YBaCo 4 O 7+δ single-crystals. At temperatures below∼80 K, a clear feature was observed which seemed to correlate with a transition into an antiferromagnetic state. Isothermal magnetization recorded at 70 K showed that field-induced effects manifested themselves through the appearance of a ferromagnetic-like component. This ferromagnetic component may arise from spin canting of the underlying antiferromagnetic state or through field-induced structural transition (at least at local scale). Although a definitive interpretation of the in

5-(2-amimo-4-styryl pyrimidine-4-yl-4-methoxybenzofuran-6-ol

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Atteyat A Labib

2013-05-01

Full Text Available This study describes the organic synthesis of 5-(2-amimo-4-styryl pyrimidine-4-yl-4-methoxy benzofuran-6-ol (SPBF as an example of a benzofuran derivative used as a new series of amyloid imaging agents. These benzofuran derivatives may be useful amyloid imaging agents for detecting B-amyloid plagues in the brain of Alzheimer’s disease. The precursor is 1-[6-hydroxy-4-methoxybenzofuran-5-yl]-phenyl butadiene ketone, which react with guanidine hydrochloride. The purification process was done via crystallization using solvent ethanol. The overall yield was 75% and the structure of the synthesized compound was confirmed by correct analytical and spectral data. Also, The synthesized compound was labeled with radioactive iodine -125 via electrophilic substitution reaction, in the presence of iodogen as an oxidizing agent, the labeling process was carried out at 95oC for 20min. The radiochemical yield was determined by using a thin layer chromatography and the yield was equal to 80%. Preliminary an in-vivo study examined normal mice after intravenous injection through the tail vein and the data showed the labeling compound was quickly cleared from most body organs. The radioiodinated compound showed high brain uptake.The results of this study suggest that radioiodinated (SPBF may be useful as a brain imaging agents.

Design of a 2.4-GHz CMOS monolithic fractional-N frequency synthesizer

Science.gov (United States)

Shu, Keliu

The wireless communication technology and market have been growing rapidly since a decade ago. The high demand market is a driving need for higher integration in the wireless transceivers. The trend is to achieve low-cost, small form factor and low power consumption. With the ever-reducing feature size, it is becoming feasible to integrate the RF front-end together with the baseband in the low-cost CMOS technology. The frequency synthesizer is a key building block in the RF front-end of the transceivers. It is used as a local oscillator for frequency translation and channel selection. The design of a 2.4-GHz low-power frequency synthesizer in 0.35mum CMOS is a challenging task mainly due to the high-speed prescaler. In this dissertation, a brief review of conventional PLL and frequency synthesizers is provided. Design techniques of a 2.4-GHz monolithic SigmaDelta fractional-N frequency synthesizer are investigated. Novel techniques are proposed to tackle the speed and integration bottlenecks of high-frequency PLL. A low-power and inherently glitch-free phase-switching prescaler and an on-chip loop filter with capacitance multiplier are developed. Compared with the existing and popular dual-path topology, the proposed loop filter reduces circuit complexity and its power consumption and noise are negligible. Furthermore, a third-order three-level digital SigmaDelta modulator topology is employed to reduce the phase noise generated by the modulator. Suitable PFD and charge-pump designs are employed to reduce their nonlinearity effects and thus minimize the folding of the SigmaDelta modulator-shaped phase noise. A prototype of the fractional-N synthesizer together with some standalone building blocks is designed and fabricated in TSMC 0.35mum CMOS through MOSIS. The prototype frequency synthesizer and standalone prescaler and loop filter are characterized. The feasibility and practicality of the proposed prescaler and loop filter are experimentally verified.

Synthesis, characterization of some novel 1,3,4-oxadiazole compounds containing 8-hydroxy quinolone moiety as potential antibacterial and anticancer agents

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Vinayak Mahadev Adimule

2014-12-01

Full Text Available In the present work a series of novel derivatives of 8-hydroxy quinolone substituted 1,3,4-oxadiazole compounds were synthesized by convergent synthetic method and studied for their antibacterial and anticancer properties. The cell lines used for cytotoxic evaluation were HeLa, Caco-2 and MCF7. The synthetic chemistry involved conversion of various substituted aromatic acids into ethyl ester 2a-e. The ethyl ester was converted into corresponding carbohydrazide 3a-e. Carbohydrazides are reacted with chloroacetic acid, phosphorous oxytrichloride and irradiated with microwave in order to obtain the various key intermediates 2-(chloromethyl-5-(substituted phenyl-1,3,4-oxadiazole 4a-e. The 2-(chloromethyl-5-(substituted phenyl-1,3,4-oxadiazole was reacted with 8-hydroxy quinolone in presence of sodium hydride and obtained a series of 8-hydroxy quinoline substituted 1,3,4-oxadiazoles 5a-e. Among the synthesised compounds, the cytotoxicity of the compound 5b i.e. 8-{[5-(2,4-dichlorophenyl-1,3,4-oxadiazol-2-yl]methoxy}quinoline against MCF7 with IC50 of 5.3µM and the compound 5e i.e. 8-{[5-(4-bromophenyl-1,3,4-oxadiazol-2-yl]methoxy}quinoline showed MIC of < 6.25µg/mL against Staphylococcus aureus which is comparable with the known standards. The standards used for cytotoxic evaluation was 5-fluorouracil and for antibacterial was nitrofurazone

Synthesized of 2,7 dihydroxyxanthone from xanthone and antimalarial activities

Science.gov (United States)

Amanatie; Jumina; Mustofa; Hanafi

2018-03-01

The purpose of the research is to synthesize 2,7-di-hydroxyxanthone compounds from xanthone and to evaluate antiplasmodial against activities. The synthesize of 2,7-di-hydroxyxanthone compounds worked with chromatogramphy methods including Thin Layer Chromatography (TLC), Vacuum Liquid Chromatography (VLC). A compound structures were determined based on the spectroscopic evidences including, Infrared (IR), one dimension (1-D) and two dimension (2-D) Nuclear Magnetic Resonance (NMR) spectra and comparison the spectroscopy data with related data from references. The biological properties of compounds are evaluated towards antiplasmodial against activity. The result of the product was obtained as white solid in 63.49% yield. The IR spectrum showed the absorption at 3433 cm-1 Which was reinforced with a sharp attack at 1087cm-1 indicating the stretching of OH, while the stretching of aromatic C=C appeared at 1620 cm-1. The 1H-NMR (500MHz, and DMSO –d6) spectrum showed that the aryl protons appeared in the region of δ12.98 ppm. In this region, there were 2 singlet at δH 12.98 ppm (1H, 2-OH) and (1H,7-OH) and shows the presence of two OH groups. Based on spectroscopy analyses, it could be started that the reaction of 2.7 di-aminoxanthone with NaNO2/HCl and H3PO4 produced 2.7-di-hydroxyxanthone. In vitro antiplasmodial assay of the product synthesized 2,7 di-hydroxyxanthones against. Falciparum strain of 3D7 showed that the IC50 values of 2,7-di-hydroxy xanthone, were 0.31 μg/mL, respectively.

Nanofibrous matrixes with biologically active hydroxybenzophenazine pyrazolone compound for cancer theranostics

International Nuclear Information System (INIS)

Kandhasamy, Subramani; Ramanathan, Giriprasath; Muthukumar, Thangavelu; Thyagarajan, SitaLakshmi; Umamaheshwari, Narayanan; Santhanakrishnan, V P; Sivagnanam, Uma Tiruchirapalli; Perumal, Paramasivan Thirumalai

2017-01-01

The nanomaterial with the novel biologically active compounds has been actively investigated for application in cancer research. Substantial use of nanofibrous scaffold for cancer research with potentially bioactive compounds through electrospinning has not been fully explored. Here, we describe the series of fabrication of nanofibrous scaffold loaded with novel potential biologically active hydroxybenzo[a]phenazine pyrazol-5(4H)-one derivatives were designed, synthesized by a simple one-pot, two step four component condensation based on Michael type addition reaction of lawsone, benzene-1,2-diamine, aromatic aldehydes and 3-methyl-1-phenyl-1H-pyrazol-5(4H)-one as the substrates. The heterogeneous solid state catalyst (Fe (III) Y-Zeolite) could effectively catalyze the reaction to obtain the product with high yield and short reaction time. The synthesized compounds (5a–5p) were analyzed by NMR, FTIR and HRMS analysis. Compound 5c was confirmed by single crystal XRD studies. All the compounds were biologically evaluated for their potential inhibitory effect on anticancer (MCF-7, Hep-2) and microbial (MRSA, MTCC 201 and FRCA) activities. Among the compounds 5i exhibited the highest levels of inhibitory activity against both MCF-7, Hep-2 cell lines. Furthermore, the compound 5i (BPP) was evaluated for DNA fragmentation, flow cytometry studies and cytotoxicity against MCF-7, Hep-2 and NIH 3T3 fibroblast cell lines. In addition, molecular docking (PDB ID: (1T46)) studies were performed to predict the binding affinity of ligand with receptor. Moreover, the synthesized BPP compound was loaded in to the PHB-PCL nanofibrous scaffold to check the cytotoxicity against the MCF-7, Hep-2 and NIH 3T3 fibroblast cell lines. The in vitro apoptotic potential of the PHB-PCL-BPP nanofibrous scaffold was assessed against MCF-7, Hep-2 cancerous cells and fibroblast cells at 12, 24 and 48 h respectively. The nanofibrous scaffold with BPP can induce apoptosis and also suppress the

Nanofibrous matrixes with biologically active hydroxybenzophenazine pyrazolone compound for cancer theranostics

Energy Technology Data Exchange (ETDEWEB)

Kandhasamy, Subramani [Organic Chemistry Division, CSIR-Central Leather Research Institute, Adyar, Chennai 600020, Tamilnadu (India); Ramanathan, Giriprasath [Bioproducts Lab, CSIR-Central Leather Research Institute, Chennai 600020, Tamilnadu (India); Muthukumar, Thangavelu [Department of Clinical and Experimental Medicine (IKE), Division of Neuro and Inflammation Sciences (NIV), Linkoping University (Sweden); Thyagarajan, SitaLakshmi [Bioproducts Lab, CSIR-Central Leather Research Institute, Chennai 600020, Tamilnadu (India); Umamaheshwari, Narayanan [Organic Chemistry Division, CSIR-Central Leather Research Institute, Adyar, Chennai 600020, Tamilnadu (India); Santhanakrishnan, V P [Department of Plant Biotechnology, TNAU, Coimbatore, Tamilnadu (India); Sivagnanam, Uma Tiruchirapalli, E-mail: suma67@gmail.com [Bioproducts Lab, CSIR-Central Leather Research Institute, Chennai 600020, Tamilnadu (India); Perumal, Paramasivan Thirumalai, E-mail: ptperumal@gmail.com [Organic Chemistry Division, CSIR-Central Leather Research Institute, Adyar, Chennai 600020, Tamilnadu (India)

2017-05-01

The nanomaterial with the novel biologically active compounds has been actively investigated for application in cancer research. Substantial use of nanofibrous scaffold for cancer research with potentially bioactive compounds through electrospinning has not been fully explored. Here, we describe the series of fabrication of nanofibrous scaffold loaded with novel potential biologically active hydroxybenzo[a]phenazine pyrazol-5(4H)-one derivatives were designed, synthesized by a simple one-pot, two step four component condensation based on Michael type addition reaction of lawsone, benzene-1,2-diamine, aromatic aldehydes and 3-methyl-1-phenyl-1H-pyrazol-5(4H)-one as the substrates. The heterogeneous solid state catalyst (Fe (III) Y-Zeolite) could effectively catalyze the reaction to obtain the product with high yield and short reaction time. The synthesized compounds (5a–5p) were analyzed by NMR, FTIR and HRMS analysis. Compound 5c was confirmed by single crystal XRD studies. All the compounds were biologically evaluated for their potential inhibitory effect on anticancer (MCF-7, Hep-2) and microbial (MRSA, MTCC 201 and FRCA) activities. Among the compounds 5i exhibited the highest levels of inhibitory activity against both MCF-7, Hep-2 cell lines. Furthermore, the compound 5i (BPP) was evaluated for DNA fragmentation, flow cytometry studies and cytotoxicity against MCF-7, Hep-2 and NIH 3T3 fibroblast cell lines. In addition, molecular docking (PDB ID: (1T46)) studies were performed to predict the binding affinity of ligand with receptor. Moreover, the synthesized BPP compound was loaded in to the PHB-PCL nanofibrous scaffold to check the cytotoxicity against the MCF-7, Hep-2 and NIH 3T3 fibroblast cell lines. The in vitro apoptotic potential of the PHB-PCL-BPP nanofibrous scaffold was assessed against MCF-7, Hep-2 cancerous cells and fibroblast cells at 12, 24 and 48 h respectively. The nanofibrous scaffold with BPP can induce apoptosis and also suppress the

Syntheses, structures and luminescence properties of lanthanide coordination polymers with helical character

International Nuclear Information System (INIS)

Zhou Ruisha; Cui Xiaobing; Song Jiangfeng; Xu Xiaoyu; Xu Jiqing; Wang Tiegang

2008-01-01

A series of lanthanide coordination polymers, (Him) n [Ln(ip) 2 (H 2 O)] n [Ln=La(1), Pr(2), Nd(3) and Dy(4), H 2 ip=isophthalic acid, im=imidazole] and [Y 2 (ip) 3 (H 2 O) 2 ] n .nH 2 O (5), have been synthesized and characterized by elemental analyses, infrared (IR), ultraviolet-visible-near infrared (UV-Vis-NIR) and single-crystal X-ray diffraction analyses. The isostructural compounds 1-4 possess 3-D structures with three different kinds of channels. Compound 5 features a 2-D network making of two different kinds of quadruple-helical chains. Compounds 2 and 3 present the characteristic emissions of Pr(III) and Nd(III) ions in NIR region, respectively. Compound 4 shows sensitized luminescence of Dy(III) ions in visible region. - Graphical abstract: A series of lanthanide coodination polymers, (Him) n [Ln(ip) 2 (H 2 O)] n [Ln=La(1), Pr(2), Nd(3) and Dy(4)] and [Y 2 (ip) 3 (H 2 O) 2 ] n .nH 2 O (5), have been reported. The isostructural compounds 1-4 possess 3-D structures with three different kinds of channels. Compound 5 displays a 2-D network making of two kinds of quadruple-helical chains. Display Omitted

Synthesis of N-(5-(Substitutedphenyl-4,5-dihydro-1H-pyrazol-3-yl-4H-1,2,4-triazol-4-amine from 4-Amino-4H-1,2,4-triazole

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Ashvin D. Panchal

2011-01-01

Full Text Available N-(4H-1,2,4-Triazol-4-ylacetamide (2 were prepared by reaction of 4-amino-4H-1,2,4-triazole (1 with acetyl chloride in dry benzene. It has been reacted with various aromatic aldehyde to afford 3-(substitutedphenyl-N-(4H-1,2,4-triazol-4-ylacrylamide (3a-e. The synthesis of N-(5-substitutedphenyl-4,5-dihydro-1H-pyrazol-3-yl-4H-1,2,4-triazol-4-amine (4a-e is achieved by the cyclisation of 3a-e with hydrazine hydrate in ethanol. The structures of synthesized compounds were characterized by 1H NMR and IR spectroscopic studies. The purity of the compounds was checked by thin layer chromatography.

Two new POMOF compounds constructed from polyoxoanions, metals and organic ligands

Science.gov (United States)

Xiao, Li-Na; Zhang, Hao; Zhang, Ting-Ting; Zhang, Xiao; Cui, Xiao-Bing

2018-03-01

Two new POMOF compounds, namely [PMo12V2O42][Cu3(4,4'-bpy)3]·(DABCO) (1) and [PMo10V4O42][Cu2(4,4'-bpy)2][Cu(phen)2]2 (2) (DABCO = triethylenediamine, bpy = bipyridine, phen = 1,10-phenanthroline)), have been synthesized and characterized by IR, UV-Vis, XRD, elemental analysis and X-ray diffraction analysis. Crystal structure analyses reveal that compounds 1 and 2 exhibit novel 2-D layered framework structures constructed from bi-capped Keggin molybdenum-vanadium polyoxoanions, metals and organic ligands, respectively. The main difference of the two compounds is that compound 2 contains both Cu2+ and Cu+ complexes. In addition, we also investigate the catalytic properties of the two compounds, both compound 1 and 2 are excellent catalysts for the epoxidation of styrene.

Synthesis and Regioselective Reaction of Some Unsymmetrical Heterocyclic Chalcone Derivatives and Spiro Heterocyclic Compounds as Antibacterial Agents.

Science.gov (United States)

El-Hashash, Maher A; Rizk, Sameh A; Atta-Allah, Saad R

2015-12-10

A number of novel heterocyclic chalcone derivatives can be synthesized by thermal and microwave tools. Treatment of 4-(4-Acetylamino- and/or 4-bromo-phenyl)-4-oxobut-2-enoic acids with hydrogen peroxide in alkaline medium were afforded oxirane derivatives 2. Reaction of the epoxide 2 with 2-amino-5-aryl-1,3,4-thiadiazole derivatives yielded chalcone of imidazo[2,1-b]thiadiazole derivative 4 via two thermal routes. In one pot reaction of 4-bromoacetophenone, diethyloxalate, and 2-amino-5-aryl-1,3,4-thiadiazole derivatives in MW irradiation (W 250 and T 150 °C) under eco-friendly conditions afforded an unsuitable yield of the desired chalcone 4d. The chalcone derivatives 4 were used as a key starting material to synthesize some new spiroheterocyclic compounds via Michael and aza-Michael adducts. The chalcone 4f was similar to the aryl-oxo-vinylamide derivatives for the inhibition of tyrosine kinase and cancer cell growth. The electron-withdrawing substituents, such as halogens, and 2-amino-1,3,4-thiadiazole moeity decreasing the electron density, thereby decreasing the energy of HOMO, and the presence of imidazothiadiazole moiety should improve the antibacterial activity. Thus, the newly synthesized compounds were evaluated for their anti-bacterial activity against (ATCC 25923), (ATCC 10987), (ATCC 274,) and (SM514). The structure of the newly synthesized compounds was confirmed by elemental analysis and spectroscopic data.

Ruthenium(II) carbonyl compounds with the 4'-chloro-2,2':6',2''-terpyridine ligand.

Science.gov (United States)

Tatikonda, Rajendhraprasad; Haukka, Matti

2017-04-01

Two ruthenium carbonyl complexes with the 4'-chloro-2,2':6',2''-terpyridine ligand (tpy-Cl, C 15 H 10 ClN 3 ), i.e. [RuCl(tpy-Cl)(CO) 2 ][RuCl 3 (CO) 3 ] (I) [systematic name: cis -di-carbonyl-chlorido(4'-chloro-2,2':6',2''-terpyridine-κ 3 N )ruthenium(II) fac -tricarbonyltri-chlorido-ruthenate(II)], and [RuCl 2 (tpy-Cl)(CO) 2 ] (II) [ cis -dicarbonyl- trans -di-chlorido(4'-chloro-2,2':6',2''-terpyridine-κ 2 N 1 , N 1' )ruthenium(II)], were synthesized and characterized by single-crystal X-ray diffraction. The Ru II atoms in both centrosymmetric structures (I) and (II) display similar, slightly distorted octa-hedral coordination spheres. The coordination sphere in the complex cation in compound (I) is defined by three N atoms of the tridentate tpy-Cl ligand, two carbonyl carbon atoms and one chlorido ligand; the charge is balanced by an octa-hedral [Ru(CO) 3 Cl 3 ] - counter-anion. In the neutral compound (II), the tpy-Cl ligand coordinates to the metal only through two of its N atoms. The coordination sphere of the Ru II atom is completed by two carbonyl and two chlorido ligands. In the crystal structures of both (I) and (II), weak C-H⋯Cl inter-actions are observed.

Synthesis, physical and chemical properties of 2-((4-R-3-(morfolinomethylen-4H-1,2,4-triazole-5-ylthioacetic acid salts

Directory of Open Access Journals (Sweden)

R. О. Shcherbyna

2017-04-01

alcohol or aqueous media the corresponding salts were obtained. Conclusions. In this study were synthesized 20 new compounds, salts of 2-((4-R-3-(morfolinometylen-4H-1,2,4-triazole-5-ylthioacetic acid. The structure of the synthesized compounds in all cases was confirmed by modern instrumental methods of analysis (1Н NMR-spectroscopy, chromatography-mass spectrometry and elemental analysis. The synthesized compounds can be used in further biological studies.

Synthesis of some new heterocyclic compounds bearing a sulfonamide moiety and studying their combined anticancer effect with γ-radiation

International Nuclear Information System (INIS)

El-Hossary, E.M.M.

2010-01-01

In search for new cytotoxic agents with improved anticancer profile, some new halogen-containing quinoline and pyrimido[4,5-b]quinoline derivatives bearing a free sulfonamide moiety were synthesized. All the newly synthesized target compounds were subjected to in vitro anticancer screening against human breast cancer cell line (MCF7). The most potent compounds, as concluded from the in vitro anticancer screening, were selected to be evaluated again for their in vitro anticancer activity in combination with radiation. Also, the newly synthesized compounds were docked in the active site of the carbonic anhydrase enzyme

Spectral characterizations and photophysical properties of one-step synthesized blue fluorescent 4′-aryl substituted 2,2′:6′,2′′-terpyridine for OLEDs application

Energy Technology Data Exchange (ETDEWEB)

Lakshmanan, Raja [Department of Physics, Birla Institute of Technology and Science, Pilani, Rajasthan 333031 (India); Shivaprakash, Narayanapura Chennegowda [Department of Instrumentation and Applied Physics, Indian Institute of Science, Bangalore 560012 (India); Nair, Sindhu Sukumaran, E-mail: sindhunair@pilani.bits-pilani.ac.in [Department of Physics, Birla Institute of Technology and Science, Pilani, Rajasthan 333031 (India)

2015-12-15

We have synthesized a series of 4′-aryl substituted 2,2′:6′,2′′-terpyridine (terpy) derivatives, namely 4′-(4-methylphenyl)-2,2′:6′,2′′-terpyridine (C-1), 4′-(2-furyl)-2,2′:6′2′′-terpyridine (C-2), and 4′-(3,4,5-trimethoxyphenyl)-2,2′:6′,2′′-terpyridine (C-3). The synthesized terpy compounds were characterized by elemental analyses, FTIR, NMR ({sup 1}H and {sup 13}C), and ESI-Mass spectrometry. Photophysical, electrochemical and thermal properties of terpy compounds were systematically studied. Maximum excitation band was observed between 240 and 330 nm using UV–visible spectra, and maximum emission peaks from PL spectra were observed at 385, 405 and 440 nm for C-1, C-2 and C-3 respectively. Fluorescence lifetime (τ) of the fluorophores was found to be 0.35 and 1.55 ns at the excitation wavelength of 406 nm for C-1 and C-2 respectively, and τ value for C-3 was found to be 0.29 ns at the excitation wavelength of 468 nm. We noticed that the calculated values of HOMO energy levels were increased from 5.96 (C-1) to 6.08 (C-3) eV, which confirms that C-3 derivative is more electrons donating in nature. The calculated electrochemical band gaps were 2.95, 2.82 and 3.02 eV for C-1, C-2 and C-3 respectively. These blue fluorescent emitter derivatives can be used as an electron transport and electroluminescent material to design the blue fluorescent organic light emitting diode (OLED) applications. - Highlights: • Facile one-step synthesized blue fluorescent emitter, 2,2′:6′,2′′-terpyridine derivatives. • The exceptionally broad emission band (365–525 nm) was achieved in the blue region. • Fast fluorescence life time and good thermal stability.

Ancillary ligand-assisted assembly of C{sub 3}-symmetric 4,4′,4″-nitrilotribenzoic acid with divalent Zn{sup 2+} ions: Syntheses, topological structures, and photoluminescence properties

Energy Technology Data Exchange (ETDEWEB)

Cui, Li-Ting; Niu, Yan-Fei [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University, 3663 North Zhongshan Road, Shanghai 200062 (China); Han, Jie, E-mail: chan@ouhk.edu.hk [School of Science & Technology, The Open University of Hong Kong, Kowloon, Hong Kong SAR (China); Zhao, Xiao-Li, E-mail: xlzhao@chem.ecnu.edu.cn [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University, 3663 North Zhongshan Road, Shanghai 200062 (China)

2015-07-15

4,4′,4″-nitrilotribenzoic acid (H{sub 3}L), a C{sub 3}-symmetric ligand, was found to self-assemble into two polymorphs driven by intermolecular hydrogen-bonding interactions. Reactions of this ligand with Zn{sup 2+} under solvothermal conditions resulted in four new coordination polymers bearing interesting structural motifs: [Zn{sub 2}(L){sub 2}(py){sub 2}]·2(H{sub 2}NMe{sub 2}){sup +}·DMF·2H{sub 2}O (1), [Zn{sub 2}(L)(H{sub 2}L)(bipy)]·1.5H{sub 2}O·Guest (2), [Zn{sub 2}(L){sub 2}(bipy)]·2(H{sub 2}NMe{sub 2}){sup +}·2DMF (3), and [Zn{sub 3}(L){sub 2}(bpa)]·2H{sub 2}O·Guest (4) (H{sub 3}L=4,4′,4′′-nitrilotribenzoic acid, DMF=dimethylformamide, py=pyridine, bipy=4,4′-bipyridine, bpa=1,2-bis(4-pyridyl)diazene). Single-crystal structural analysis revealed that compound 1 exhibits a rare example of twofold interpenetrating anionic 3D (3,3)-net framework containing helical channels, whereas in 2, the 3D pillar-layer structure generated from bipy-pillared Zn{sub 2}(L)(H{sub 2}L) layer is further reinforced by intermolecular hydrogen bonding among pairs of free –COOH units. Compound 3 shows an interesting entangled architecture of 2D→3D parallel polycatenation consisting five-coordinated Zn{sup 2+} ions. Compound 4 displays a 3D pillar-layer framework with trimeric Zn{sub 3}(CO{sub 2}){sub 6} serving as secondary building unit (SBU). The syntheses, structures, thermal stabilities, powder X-ray diffractions and solid-state photoluminescence properties for these crystalline materials have been carried out. In addition, supramolecular assembly of H{sub 3}L under solvothermal conditions will also be addressed. - Graphical abstract: Supramolecular assembly of 4,4′,4′′-nitrilotribenzoic acid and its ligand behavior toward Zn{sup 2+} were investigated, which exhibit two polymorphs of the free acid and four metal coordination polymers bearing interesting structural motifs. - Highlights: • Two polymorphs of H{sub 3}L showing different hydrogen

Design and syntheses of mono and multivalent mannosyl-lipoconjugates for targeted liposomal drug delivery.

Science.gov (United States)

Štimac, Adela; Cvitaš, Jelena TrmĿiĿ; Frkanec, Leo; Vugrek, Oliver; Frkanec, Ruža

2016-09-10

Multivalent mannosyl-lipoconjugates may be of interest for glycosylation of liposomes and targeted drug delivery because the mannose specifically binds to C-type lectin receptors on the particular cells. In this paper syntheses of two types of novel O-mannosides are presented. Conjugates 1 and 2 with a COOH- and NH2-functionalized spacer and the connection to a lysine and FmocNH-PEG-COOH, are described. The coupling reactions of prepared intermediates 6 and 4 with a PEGylated-DSPE or palmitic acid, respectively, are presented. Compounds 5, mono-, 8, di- and 12, tetravalent mannosyl-lipoconjugates, were synthesized. The synthesized compounds were incorporated into liposomes and liposomal preparations featuring exposed mannose units were characterized. Carbohydrate liposomal quartz crystal microbalance based assay has been established for studying carbohydrate-lectin binding. It was demonstrated that liposomes with incorporated mannosyl-lipoconjugates were effectively recognized by Con A and have great potential to be used for targeted liposomal drug delivery systems. Copyright © 2016 Elsevier B.V. All rights reserved.

Biological and Docking Studies of Sulfonamide Derivatives of 4-Aminophenazone

International Nuclear Information System (INIS)

Akhtar, M.S.; Ismail, A.; Murtaza, S.; Shamim, S.; Tahir, M.N.; Usman Ali Rana, U.A.

2016-01-01

Sulfonamide derivatives of 4-aminophenazone (4APZ) were synthesized and accordingly characterized by spectroscopic techniques. These newly synthesized compounds were examined for their biological activities such as enzyme inhibition, analgesic, antibacterial, antioxidant and DNA interaction. A direct correlation between enzyme inhibition activity and concentration of the compounds was observed both by experimental and molecular docking studies. Analgesic activity of the compounds was investigated by formalin-induced paw licking (FIPL), acetic acid-induced writhing (AIW) and heat conduction methods in mice. Membrane stabilization effect was determined by hypotonicity-induced hemolysis. Bacterial strains, S. aureus, S. epidermidis, B. subtilis, E. coli, P. aeruginosa, S. mutans and A. odontolyticus were used for investigating the antibacterial potential of the compounds. Antioxidant potential was investigated by Ferric Reducing Antioxidant Power assay (FRAP) and DPPH free radical scavenging method. DNA interaction studies of the synthesized compounds showed weak interaction. Hyperchromic effect was observed along the series and large positive K values were obtained for most of the compounds. (author)

Synthesis, characterization and biological evaluation of novel diesters of 4,4'-dihydroxy azoxy benzene with long chain carboxylic acid

International Nuclear Information System (INIS)

Shehzadi, S.; Siddiqi, H.M.; Qasim, M.M.

2014-01-01

Synthesis of novel symmetrical azoxy diesters have been prepared by the reaction of 4,4'-dihydroxyazoxy benzene with aliphatic acid halides of varying chain lengths. The synthesized compounds have been characterized by spectral and analytical means. These symmetrical azoxy diesters exhibit good antifungal against six fungal strains (Mucor species, Aspergillus niger, Aspergillus flavus, Alternaria solani, Fusarium solani and Aspergillus fumigatus) and antitumor activities while no significant antibacterial activity has been observed. These synthesized compounds are also potent free radical scavengers. (author)

Cobalt, nickel and cadmium coordination compounds with phenylacetylhydrazine

Energy Technology Data Exchange (ETDEWEB)

Machkhoshvili, R.I.; Metreveli, D.P.; Mitaishvili, G.Sh.; Shchelokov, R.N.

1985-03-01

In the process of interaction of aqueous-ethanol solutions of chlorides, sulphates, nitrates, thiocyanates of cobalt, nickel, cadmium and phenylacetylhydrazine in neutral or low-acid medium coordination compounds: (M(EAG)/sub 3/)X/sub 2/ (M=Co, Ni; X=Cl, 1/2SO/sub 4/, NO/sub 3/), Cd(FAG)/sub 2/X/sub 2/ (X = Cl, 1/2SO/sub 4/, NCS), Ni(EAG)/sub 2/(NCS)/sub 2/, where FAG C/sub 6/H/sub 5/CH/sub 2/xCONHNH/sub 2/, have been synthesized. In the reactions of aqueous-ethanol solutions of (Co(NH/sub 3/)/sub 5/Cl)Cl/sub 2/ and phenylacetylhydrazine the complex Co(C/sub 6/H/sub 5/CH/sub 2/CONNH/sub 2/)/sub 3/ is prepared. Certain physicochemical properties and IR absorption spectra of the coordination compounds synthesized are studied.

Water linked 3D coordination polymers: Syntheses, structures and applications

Energy Technology Data Exchange (ETDEWEB)

Singh, Suryabhan, E-mail: sbs.bhu@gmail.com; Bhim, Anupam

2016-12-15

Three new coordination polymers (CPs) based on Cd and Pb, [Cd(OBA)(μ-H{sub 2}O)(H{sub 2}O)]{sub n}1, [Pb(OBA)(μ-H{sub 2}O)]{sub n}2 [where OBA=4,4’-Oxybis(benzoate)] and [Pb(SDBA)(H{sub 2}O)]{sub n}.1/4DMF 3 (SDBA=4,4’-Sulfonyldibenzoate), have been synthesized and characterized. The single crystal structural studies reveal that CPs 1 and 2 have three dimensional structure. A water molecule bridges two metal centres which appears to the responsible for the dimensionality increase from 2D to 3D. Compound 3 has a supramolecular 3D structure involving water molecule and hydrogen bonds. A structural transformation is observed when 3 was heated at 100 °C or kept in methanol, forming [Pb(SDBA)]{sub n}4. Compound 4 is used as supporting matrix for palladium nanoparticles, PdNPs@4. The PdNPs@4 exhibits good catalytic activity toward the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the presence of NaBH{sub 4} at room temperature. Luminescence studies revealed that all CPs could be an effective sensor for nitroaromatic explosives. - Graphical abstract: Three new CPs based on Cd and Pb, have been synthesized and characterized. A water molecule bridges two metal centres which appears to the responsible for the dimensionality increase from 2D to 3D. One of the CP is used as supporting matrix for palladium nanoparticles, PdNPs@4. The PdNPs@4 exhibits good catalytic activity toward the reduction of 4-nitrophenol. Luminescence studies shown that all CPs could be an effective sensor for nitroaromatic explosives. - Highlights: • Three new CPs based on Cd and Pb, have been synthesized and characterized. • A water molecule bridges two metal centres which appears to the responsible for the dimensionality increase from 2D to 3D. • One of the CP is used as supporting matrix for palladium nanoparticles, PdNPs@4. • Luminescence studies shown that all CPs could be an effective sensor for nitroaromatic explosives.

Synthesis and Evaluation of the Anticonvulsant Activities of 4-(2-(Alkylthiobenzo[d]oxazol-5-yl-2,4-dihydro-3H-1,2,4-triazol-3-ones

Directory of Open Access Journals (Sweden)

Ming-Xia Song

2018-03-01

Full Text Available In this study, a novel series of 4-(2-(alkylthiobenzo[d]oxazol-5-yl-2,4-dihydro-3H-1,2,4-triazol-3-ones (4a–m was designed and synthesized. The anticonvulsant activities of these compounds were evaluated by using the maximal electroshock seizure (MES and subcutaneous pentylenetetrazole (scPTZ seizure models in mice. The neurotoxicity of these compounds was evaluated using the rotarod neurotoxicity test. The majority of compounds showed anti-MES activities at 100 or 300 mg/kg. Compound 4g was considered to be the most promising, based on its potency against MES- and PTZ-induced seizures with ED50 values of 23.7 and 18.9 mg/kg, respectively. The TD50 value of 4g was 284.0 mg/kg, which resulted in a higher protective index (PI = TD50/ED50 value than that of carbamazepine and valproate. In an ELISA test, compound 4g significantly increased the γ-aminobutyric acid (GABA content in mouse brain. In addition, pretreatment with thiosemicarbazide (an inhibitor of the GABA synthesizing enzyme significantly decreased the activity of 4g in the MES model, which suggests that the mechanism through which compound 4g elicits its anticonvulsive action is at least in part through increasing the GABA level in the brain.

Synthesis and characterization of new oxides and oxynitrides of niobium; Synthese und Charakterisierung neuer Oxide und Oxidnitride des Niobs

Energy Technology Data Exchange (ETDEWEB)

Orthmann, Steven

2017-11-02

By different synthesis routes the first oxide nitrides in the series scandium-niobium-oxygen-nitrogen could be synthesized and characterized. ScNb{sub 4}O{sub 7}N{sub 3}, which crystallizes in the rutile-type structure, exhibit a band gap of 2.62 eV after a short oxidation. Furthermore anion-deficit NbSc{sub 2}(O,N,□){sub 6} with fluorite-type structure could be synthesized. UV-Vis measurements point to a band gap of 3.36 eV after a short oxidation of the product. In the series zirconium-niobium-oxygen-nitrogen new oxides and oxide nitrides could be synthesized. By replacing zirconium with hafnium isotopical compounds with comparable composition could be obtained. The crystal structure of these new compounds is discussed respecting magnetism and the results of electron microscopy and neutron diffraction. By partially substitution of niobium with magnesium or zinc three additional oxide nitrides with the compositions Mg{sub 2}Nb{sub 4}O{sub 2}N{sub 5}, Zn{sub 2}NbO{sub 0,3}N{sub 2,8}, and ZnNb{sub 3}O{sub 0,1}N{sub 4,5}, showing a tetragonal Nb{sub 4}N{sub 5}-type structure, could be synthesized.

Synthesis, pharmacological activity evaluation and molecular modeling of new polynuclear heterocyclic compounds containing benzimidazole derivatives.

Science.gov (United States)

Bassyouni, Fatma A; Saleh, Tamer S; ElHefnawi, Mahmoud M; Abd El-Moez, Sherein I; El-Senousy, Waled M; Abdel-Rehim, Mohamed E

2012-12-01

Novel heterocyclic compounds containing benzimidazole derivatives were synthesized from 2-(1H-benzimidazol-2-yl) acetonitrile (1) and arylhydrazononitrile derivative 2 was obtained via coupling of 1 with 4-methyl phenyldiazonium salt, which was then reacted with hydroxylamine hydrochloride to give amidooxime derivative 3. This product was cyclized into the corresponding oxadiazole derivative 4 upon reflux in acetic anhydride. Compound 4 was refluxed in DMF in the presence of triethylamine to give the corresponding 5-(1H-benzimidazol-2-yl)-2-p-tolyl-2H-1,2,3-triazol-4-amine 6. Treatment of compound 6 with ethyl chloroformate afforded 2,6-dihydro-2-(4-methylphenyl)-1,2,3-triazolo[4",5"-4',5']pyrimido[1,6-a]benzimidazole-5(4H)-one (8). 1,2-bis(2-cyanomethyl-1H-benzimidazol-1-yl)ethane-1,2-dione (10) was synthesized via the condensation reaction of 2-(1H-benzimidazol-2-yl) acetonitrile (1) and diethyloxalate. The reactivity of compound 10 towards some diamine reagents was studied. The in vitro antimicrobial activity of the synthesized compounds was investigated against several pathogenic bacterial strains such as Escherichia coli O157, Salmonella typhimurium, E. coli O119, S. paratyphi, Pseudomonas aeruginosa, Staphylococcus aureus, Listeria monocytogenes and Bacillus cereus. The results of MIC revealed that compounds 12a-c showed the most effective antimicrobial activity against tested strains. On the other hand, compounds 12a, b exhibited high activity against rotavirus Wa strain while compounds 12b, c exhibited high activity against adenovirus type 7. In silico target prediction, docking and validation of the compounds 12a-c were performed. The dialkylglycine decarboxylase bacterial enzyme was predicted as a potential bacterial target receptor using pharmacophore-based correspondence with previous leads; giving the highest normalized scores and a high correlation docking score with mean inhibition concentrations. A novel binding mechanism was predicted after docking

Effect of lead salts on phase, morphologies and photoluminescence of nanocrystalline PbMoO4 and PbWO4 synthesized by microwave radiation

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Phuruangrat Anukorn

2016-09-01

Full Text Available PbMoO4 and PbWO4 were successfully synthesized by microwave radiation using different lead salts (acetate, chloride, nitrate and sulfate and Na2MO4 (M = Mo, W in propylene glycol. The products were characterized by X-ray diffraction (XRD, scanning and transmission electron microscopy (SEM, TEM, Fourier transform infrared (FT-IR, Raman spectroscopy and photoluminescence (PL spectroscopy. In this research, morphologies, crystallization and photoluminescence of the products were influenced by the kinetics of anions, including the detection of M–O (M = Mo, W stretching modes in the (MO42− tetrahedrons. Photoluminescence of PbMoO4 synthesized from Pb(NO32 and of PbWO4 synthesized from PbCl2 showed the strongest blue emission due to the electronic diffusion in tetrahedrons at room temperature.

Enhanced thermoelectric properties of N-type polycrystalline In4Se3-x compounds via thermally induced Se deficiency

Science.gov (United States)

Zhao, Ran; Shu, Yu-Tian; Guo, Fu

2014-03-01

In4Se3-x compound is considered as a potential thermoelectric material due to its comparably low thermal conductivity among all existing ones. While most studies investigated In4Se3-x thermoelectric properties by controlling selennium or other dopants concentrations, in the current study, it was found that even for a fixed initial In/Se ratio, the resulting In/Se ratio varied significantly with different thermal processing histories (i.e., melting and annealing), which also resulted in varied thermoelectric properties as well as fracture surface morphologies of In4Se3-x polycrystalline specimens. Single phase polycrystalline In4Se3-x compounds were synthesized by combining a sequence of melting, annealing, pulverizing, and spark plasma sintering. The extension of previous thermal history was observed to significantly improve the electrical conductivity (about 121%) and figure of merit (about 53%) of In4Se3-x polycrystalline compounds. The extended thermal history resulted in the increase of Se deficiency (x) from 0.39 to 0.53. This thermally induced Se deficiency was observed to associate with increasing carrier mobility but decreasing concentration, which differs from the general trend observed for the initially adjusted Se deficiency at room temperature. Unusually large dispersed grains with nanosize layers were observed in specimens with the longest thermal history. The mechanism(s) by which previous thermal processing enhances carrier mobility and affect microstructural evolution are briefly discussed.

Copper(II) complexes with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid: Syntheses, crystal structures and antifungal activities

International Nuclear Information System (INIS)

Xiong, Pingping; Li, Jie; Bu, Huaiyu; Wei, Qing; Zhang, Ruolin; Chen, Sanping

2014-01-01

Reaction of Cu(II) with an asymmetric semi-rigid organic ligand 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid (HL), yielded five compounds, [Cu 0.5 L] n (1), [Cu(HL) 2 Cl 2 ] n (2), [Cu(HL) 2 Cl 2 (H 2 O)] (3), [Cu(L) 2 (H 2 O)] n (4) and [Cu(L)(phen)(HCO 2 )] n (5), which have been fully characterized by infrared spectroscopy, elemental analysis, and single-crystal X-ray diffraction. As for compounds 1, 2 and 5, Cu(II) is bridged through HL, Cl - , and formic acid, respectively, featuring 1D chain-structure. In compound 3, Cu(II) with hexahedral coordination sphere is assembled through hydrogen-bonding into 3D supramolecular framework. In compound 4, 1D chain units –Cu–O–Cu–O– are ligand-bridged into a 3D network. All compounds were tested on fungi (Fusarium graminearum, Altemaria solani, Macrophoma kawatsukai, Alternaria alternata and Colletotrichum gloeosporioides). Compound 1 exhibits a better antifungal effect compared to other compounds. An effect of structure on the antifungal activity has also been correlated. - Graphical abstract: Copper(II) compounds with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid, were prepared, structurally characterized and investigated for antifungal activity. - Highlights: • The title compounds formed by thermodynamics and thermokinetics. • The five compounds show higher inhibition percentage than reactants. • The structure effect on the antifungal activity

Synthesis of tetravalent actinide chlorides. Versatile compounds for actinide chemistry

Energy Technology Data Exchange (ETDEWEB)

Maerz, Juliane [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Div. Chemistry of the F-Elements

2016-07-01

Anhydrous actinide tetrachlorides (AnCl{sub 4}) were synthesized under mild conditions to provide versatile compounds for actinide chemistry. They enable a direct access to actinide complexes with organic and inorganic ligands.

Studies on the effect of a newly synthesized Schiff base compound from phenazone and vanillin on the corrosion of steel in 2M HCl

International Nuclear Information System (INIS)

Emreguel, Kaan C.; Hayvali, Mustafa

2006-01-01

The inhibiting action of a Schiff base 4-[(4-hydroxy-3-hydroxymethyl-benzylidene)-amino]-1,5-dimethyl-2-phenyl-1,2 -dihydro-pyrazol-3-one (phv), derived from 4-amino-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-one (phz) and 4-hydroxy-3-methoxy-benzaldehyde (vn), towards the corrosion behavior of steel in 2M HCl solution has been studied using weight loss, polarization and electrochemical impedance spectroscopy (EIS) techniques. Although vn and phz were found to retard the corrosion rate of steel, the compound synthesized from vn and phz was seen to retard the corrosion rate even more. At constant temperature, the corrosion rate decreases with increasing inhibitor concentration. However, at any inhibitor concentration the increase in temperature leads to an increase in the corrosion rate of steel. The activations energies, ΔE a , as well as other thermodynamic parameters (ΔG ads 0 , ΔH ads 0 ) for the inhibitor process were calculated. The inhibitor efficiencies calculated from all the applied methods were in agreement and were found to be in the order: phv>phz>vn

Copper(II) complexes with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid: Syntheses, crystal structures and antifungal activities

Energy Technology Data Exchange (ETDEWEB)

Xiong, Pingping [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China); Li, Jie [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Bu, Huaiyu, E-mail: 7213792@qq.com [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Wei, Qing [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China); Zhang, Ruolin [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Chen, Sanping, E-mail: sanpingchen@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China)

2014-07-01

Reaction of Cu(II) with an asymmetric semi-rigid organic ligand 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid (HL), yielded five compounds, [Cu{sub 0.5}L]{sub n} (1), [Cu(HL){sub 2}Cl{sub 2}]{sub n} (2), [Cu(HL){sub 2}Cl{sub 2}(H{sub 2}O)] (3), [Cu(L){sub 2}(H{sub 2}O)]{sub n} (4) and [Cu(L)(phen)(HCO{sub 2})]{sub n} (5), which have been fully characterized by infrared spectroscopy, elemental analysis, and single-crystal X-ray diffraction. As for compounds 1, 2 and 5, Cu(II) is bridged through HL, Cl{sup -}, and formic acid, respectively, featuring 1D chain-structure. In compound 3, Cu(II) with hexahedral coordination sphere is assembled through hydrogen-bonding into 3D supramolecular framework. In compound 4, 1D chain units –Cu–O–Cu–O– are ligand-bridged into a 3D network. All compounds were tested on fungi (Fusarium graminearum, Altemaria solani, Macrophoma kawatsukai, Alternaria alternata and Colletotrichum gloeosporioides). Compound 1 exhibits a better antifungal effect compared to other compounds. An effect of structure on the antifungal activity has also been correlated. - Graphical abstract: Copper(II) compounds with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid, were prepared, structurally characterized and investigated for antifungal activity. - Highlights: • The title compounds formed by thermodynamics and thermokinetics. • The five compounds show higher inhibition percentage than reactants. • The structure effect on the antifungal activity.

Synthesis, herbicidal, fungicidal and insecticidal evaluation of 3-(dichlorophenyl)- isocoumarins and (±)-3-(dichlorophenyl)-3,4-dihydroisocoumarins

International Nuclear Information System (INIS)

Qadeer, Ghulam; Rama, Nasim Hasan; Fan, Zhi-Jin; Liu, Bin; Liu, Xiu-Feng

2007-01-01

This is the first report showing that 3-(dichlorophenyl)isocoumarins and (±)-3,4-dihydroisocoumarins are plant and plant fungus growth inhibitors. 3-Dichlorophenylisocoumarins were synthesized by condensation of homophthalic acid with dichlorobenzoyl chlorides. The alkaline hydrolysis of these isocoumarins afforded keto acids. Racemic 3-(Dichlorophenyl)-3,4-dihydroisocoumarins were obtained by reduction of keto acids to racemic hydroxy acids, followed by cyclodehydration using acetic anhydride. The herbicidal, fungicidal and insecticidal activities of the synthesized compounds have been evaluated. Some of the synthesized compounds show excellent herbicidal and fungicidal activities but none of the synthesized compounds presented any insecticidal effects on the test insects. The findings of this study suggest that isocoumarins and related compounds may serve as lead compounds towards the design of bioactive herbicides and fungicides. (author)

Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized {sup 118}Sn-enriched organotin compounds

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi [National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, National Metrology Institute of Japan (NMIJ), Tsukuba, Ibaraki (Japan)

2007-04-15

A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with {gamma}-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS) - SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with {sup 118}Sn-enriched organotin compounds synthesized from {sup 118}Sn-enriched metal used as a spike. The {sup 118}Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the {sup 118}Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44{+-}3 {mu}g kg{sup -1} as Sn, DBT 51 {+-} 2 {mu}g kg{sup -1} as Sn, MBT 67 {+-} 3 {mu}g kg{sup -1} as Sn, TPhT 6.9 {+-} 1.2 {mu}g kg{sup -1} as Sn, and DPhT 3.4 {+-} 1.2 {mu}g kg{sup -1} as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. (orig.)

(3,5-Dimethylpyrazol-1-yl-[4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminophenyl]methanone

Directory of Open Access Journals (Sweden)

Rania B. Bakr

2016-11-01

Full Text Available In an attempt to enhance cytotoxic activity of pyrazolo[3,4-d]pyrimidine core, we synthesized (3,5-dimethylpyrazol-1-yl-[4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminophenyl]methanone (4 by reacting 4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminobenzohydrazide (3 with acetylacetone. Antiproliferative activity of this compound was screened against breast (MCF-7, colon (HCT-116, and liver (HEPG-2 cancer cell lines. The tested compound exhibited cytotoxic activity with IC50 = 5.00–32.52 μM. Moreover, inhibitory activity of this compound was evaluated against the epidermal growth factor receptor (EGFR, the fibroblast growth factor receptor (FGFR, the insulin receptor (IR, and the vascular endothelial growth factor receptor (VEGFR. This target compound showed potent inhibitory activity, especially against FGFR with IC50 = 5.18 μM.

Syntheses, structures and photoluminescent properties of Zn(Ⅱ)/Co(Ⅱ) coordination polymers based on flexible tetracarboxylate ligand of 5,5′-(butane-1,4-diyl)-bis(oxy)-di isophthalic acid

Energy Technology Data Exchange (ETDEWEB)

Gao, Yan-Peng [Inner Mongolia Key Lab Chem & Phys Rare Earth Mat, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Department of Chemistry and Chemical Engineering, Ordos College of Inner Mongolia University, Ordos 017000 (China); Department of Chemistry and Chemical Engineering, Ordos Applied Technology College, Ordos 017000 (China); Guo, Le [Department of Chemistry and Chemical Engineering, Ordos College of Inner Mongolia University, Ordos 017000 (China); Department of Chemistry and Chemical Engineering, Ordos Applied Technology College, Ordos 017000 (China); Dong, Wei; Jia, Min; Zhang, Jing-Xue; Sun, Zhong [Inner Mongolia Key Lab Chem & Phys Rare Earth Mat, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Chang, Fei, E-mail: ndchfei@imu.edu.cn [Inner Mongolia Key Lab Chem & Phys Rare Earth Mat, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China)

2016-08-15

Three new mixed-ligand metal-organic frameworks based on 5,5′-(butane-1,4- diyl)-bis(oxy)-diisophthalic acid and transitional metal cations with the help of two ancillary bridging N-donor pyridyl and imidazole linkers, [Zn(L){sub 0.5}(4,4′-bpy)]·2(H{sub 2}O) (1), [M(L){sub 0.5}(bib)]·4(H{sub 2}O) (M = Zn (2), Co (3)), (4,4′-bpy=4,4′–bipyridine, bib=1,4-bis (1H-imidazol-1-yl)-butane), have been synthesized under solvothermal conditions. Their structures and properties were determined by single-crystal and powder X-ray diffraction analyses, IR spectra, elemental analyses and thermogravimetric analyses (TGA). Compounds 1–3 display a 3D 3-fold interpenetrated frameworks linked by the L{sup 4−} ligands, ancillary N-donor linkers and the free water molecules in the crystal lattice. Topological analysis reveals that 1–3 are a (4,4)-connected bbf topology net with the (6{sup 4}·8{sup 2})(6{sup 6}) topology. The effects of the L{sup 4−} anions, the N-donor ligands, and the metal ions on the structures of the coordination polymers have been discussed. Furthermore, luminescence properties and thermogravimetric properties of these compounds were investigated. - Graphical abstract: Three new compounds of MOFs have been prepared and characterized. The luminescence properties and thermogravimetric properties of compounds were investigated. Display Omitted.

Synthesis, Characterization, and Biological Activity of Novel Schiff and Mannich Bases of 4-Amino-3-(N-phthalimidomethyl-1,2,4-triazole-5-thione

Directory of Open Access Journals (Sweden)

Uzma Yunus

2013-01-01

Full Text Available The present work describes the syntheses and antimicrobial activity studies of a series of novel Schiff bases (4a–4i and their Mannich bases (5a–5h starting from 4-amino-3-(N-phthalimido-methyl-1,2,4-triazole-5-thione (3. All the synthesized compounds were characterized by IR, 1H-NMR, 13C-NMR, and MS. All the synthesized compounds were screened for four Gram-negative strains, one Gram-positive strain of bacteria, and one diploid fungal strain. In general the antimicrobial activity increased remarkably on the introduction of azomethine functionality in parent triazole (3. The antimicrobial activity further improved when morpholine group was added to them except for Enterobacter cloacae, where loss of activity was observed. The results are promising and show that the fine tuning of the structures (5a, 5b, 5e, 5f, and 5h can lead to some new antimicrobial compounds.

Complexing Agents on Carbon Content and Lithium Storage Capacity of LiFePO4/C Cathode Synthesized via Sol-Gel Approach

Directory of Open Access Journals (Sweden)

C. Guan

2016-01-01

Full Text Available Olivine-structured LiFePO4 faces its intrinsic challenges in terms of poor electrical conductivity and lithium-ion diffusion capability for application to lithium-ion batteries. Cost-effective sol-gel approach is advantageous to in situ synthesize carbon-coated LiFePO4 (LiFePO4/C which can not only improve electronic conductivity but also constrain particle size to nanometer scale. In this study, the key parameter is focused on the choice and amount of chelating agents in this synthesis route. It was found that stability of complexing compounds has significant impacts on the carbon contents and electrochemical properties of the products. At the favorable choice of precursors, composition, and synthesis conditions, nanocrystalline LiFePO4/C materials with appropriate amount of carbon coating were successfully obtained. A reversible capacity of 162 mAh/g was achieved at 0.2C rate, in addition to good discharge rate capability.

Noval 1-substituted-3,5-dimethyl-4-[(substituted phenyl diazenyl] pyrazole derivatives: Synthesis and pharmacological activity

Directory of Open Access Journals (Sweden)

Sabir Hussain

2015-05-01

Full Text Available Several-1-carbothioamide-3,5-dimethyl-4-[(substituted phenyl diazenyl] pyrazoles 2a–d, 1-(pyridine-4-ylcarbonyl-3,5-dimethyl-4-[(substituted phenyl diazenyl] pyrazoles 3a–d, 1-(5-chloro-6-fluoro-1,3-benzothiazole-2-ylthiocarbamoyl-3,5-dimethyl-4-[(substituted phenyl diazenyl] pyrazoles 4a–d and 1-[(1,2,4-triazole-4-yl carbothioamide]-3,5-dimethyl-4-[(substituted phenyl diazenyl] pyrazoles 5a–d were synthesized. The structures of the newly synthesized compounds were supported by IR, 1H NMR and mass spectral data. These compounds were investigated for their, anti-inflammatory, analgesic, ulcerogenic, lipid peroxidation, antibacterial and antifungal activities. Some of the synthesized compounds showed potent anti-inflammatory activity along with minimal ulcerogenic effect and lipid peroxidation, compared to ibuprofen and flurbiprofen. Some of the tested compounds also showed moderate antimicrobial activity against tested bacterial and fungal strains.

Design, synthesis and pharmacological evaluation of some novel derivatives of 1-{[3-(furan-2-yl-5-phenyl-4,5-dihydro-1,2-oxazol-4-yl]methyl}-4-methyl piperazine

Directory of Open Access Journals (Sweden)

Jagdish Kumar

2017-01-01

Full Text Available A novel series of 1-{[3-(furan-2-yl-5-substituted phenyl-4,5-dihydro-1,2-oxazol-4-yl]methyl}-4-methyl piperazine, compounds 3a–l have been synthesized. The synthetic work was carried out beginning from 2-acetylfuran through Claisen Schmidt condensation with different types of aromatic aldehyde, affording 1-(furan-2-yl-3-substitutedphenylprop-2-en-1-ones which on cyclization with hydroxylamine hydrochloride resulted in 3-(furan-2-yl-5-substitutedphenyl-4,5-dihydro-1,2-oxazole formation. The isoxazolines were subjected to Mannich’s reaction in the presence of N-methyl piperazine to produce the desired product. The chemical structures of the compounds were proved by IR, 1H NMR, 13C-NMR and Mass spectrometric data. The antidepressant activities of the compounds were investigated by Porsolt’s behavioral despair (forced swimming test on albino mice. Moreover, the antianxiety activity of the newly synthesized compounds was investigated by the plus maze method. Compounds 3a and 3k reduced the duration of immobility times of 152.00–152.33% at 10 mg/kg dose level and compounds 3a and 3k have also shown significant antianxiety activity.

Design and syntheses of novel N-(benzothiazol-5-yl)-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-dione and N-(benzothiazol-5-yl)isoindoline-1,3-dione as potent protoporphyrinogen oxidase inhibitors.

Science.gov (United States)

Jiang, Li-Li; Zuo, Yang; Wang, Zhi-Fang; Tan, Yin; Wu, Qiong-You; Xi, Zhen; Yang, Guang-Fu

2011-06-08

Discovery of protoporphyrinogen oxidase (PPO, EC 1.3.3.4) inhibitors has been one of the hottest research areas in the field of herbicide development for many years. As a continuation of our research work on the development of new PPO-inhibiting herbicides, a series of novel N-(benzothiazol-5-yl)-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-diones (1a-p) and N-(benzothiazol-5-yl)isoindoline-1,3-diones (2a-h) were designed and synthesized according to the ring-closing strategy of two ortho-substituents. The bioassay results indicated that some newly synthesized compounds exhibited higher PPO inhibition activity than the control of sulfentrazone. Compound 1a, S-(5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl) O-methyl carbonothioate, was identified as the most potent inhibitor with k(i) value of 0.08 μM, about 9 times higher than that of sulfentrazone (k(i) = 0.72 μM). Further green house assay showed that compound 1b, methyl 2-((5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl)thio)acetate, exhibited herbicidal activity comparable to that of sulfentrazone even at a concentration of 37.5 g ai/ha. In addition, among six tested crops, wheat exhibited high tolerance to compound 1b even at a dosage of 300 g ai/ha. These results indicated that compound 1b might have the potential to be developed as a new herbicide for weed control of wheat field.

Synthesis of 4-aryl-2,6-dimethyl-3,5-bis-N-(aryl-carbamoyl-1,4-dihydropyridines as novel skin protecting and anti-aging agents

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Aamer Saeed

2017-06-01

Full Text Available A series of 4-aryl-2,6-dimethyl-3,5-bis-N-(aryl-carbamoyl-1,4-dihydropyri-dines 6a-6h were prepared by using the one-pot three component synthetic method. The target compounds 6a-6h were synthesized by reacting two molar equivalents of ketone functionality and one mole of aromatic aldehydes in ammonium acetate to obtain the desired products. The structures of newly synthesized compounds were characterized by FT-IR, 1H-NMR, 13C-NMR, and elemental analysis. All the synthesized compounds were screened for their elastase inhibition and antioxidant activity. Almost all of the com-pounds 6a-h showed good to excellent activities against elastase enzyme more than the reference drug. Compounds 6d and 6b at 0.2 ± 0.0 µM and 0.2 ± 0.0 µM were found to most potent derivatives against elastase enzyme. Compound 6a exhibited prominent free radical scavenging activity. From the results of the biological activity, we infer that some derivatives can serve as lead molecules in pharmacology.

Synthesis and 5α-Reductase Inhibitory Activity of C21 Steroids Having 1,4-diene or 4,6-diene 20-ones and 4-Azasteroid 20-Oximes

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Eunsook Ma

2011-12-01

Full Text Available The synthesis and evaluation of 5α-reductase inhibitory activity of some 4-azasteroid-20-ones and 20-oximes and 3β-hydroxy-, 3β-acetoxy-, or epoxy-substituted C21 steroidal 20-ones and 20-oximes having double bonds in the A and/or B ring are described. Inhibitory activity of synthesized compounds was assessed using 5α-reductase enzyme and [1,2,6,7-3H]testosterone as substrate. All synthesized compounds were less active than finasteride (IC50: 1.2 nM. Three 4-azasteroid-2-oximes (compounds 4, 6 and 8 showed good inhibitory activity (IC50: 26, 10 and 11 nM and were more active than corresponding 4-azasteroid 20-ones (compounds 3, 5 and 7. 3β-Hydroxy-, 3β-acetoxy- and 1α,2α-, 5α,6α- or 6α,7α-epoxysteroid-20-one and -20-oxime derivatives having double bonds in the A and/or B ring showed no inhibition of 5α-reductase enzyme.

Synthesis, characterization and anti cancer activity of some fluorinated 3,6-diaryl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazoles

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Deepak Chowrasia

2017-05-01

Full Text Available A series of fluorinated 3,6-diaryl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazoles (2a–2i was synthesized by condensation of various substituted 4-amino-5-phenyl-4H-1,2,4-triazole-3-thiols (1a–1i with penta fluoro benzoic acid in good yields (60–80%. The synthesized compounds were screened for anticancer activity against three cancerous cell lines MCF7 (human breast cancer, SaOS-2 (human osteosarcoma and K562 (human myeloid leukemia. The compounds showed moderate to good antiproliferative potency against the studied cell lines. Among these, compound 2b showed higher antiproliferative activity (IC50 22.1, 19 and 15 μM against MCF7, SaOS-2 and K562, respectively while 2a exhibited least antiproliferative activity (IC50 30.2, 39 and 29.4 μM against MCF7, SaOS-2 and K562 cells, respectively. Therefore, the present study demonstrates that fluorine substituted 3,6-diaryl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazoles would be a better prospective in the development of anticancer drugs.

Magnetic response of polycrystalline YBaCo{sub 4}O{sub 7+δ} synthesized through the physical and chemical route: The role of phase inhomogeneities

Energy Technology Data Exchange (ETDEWEB)

Vallejos, E. [Universidad de Nariño, Centro de Materiales Avanzados, Torobajo, Pasto (Colombia); Galeano, V.; Gómez, L.; Izquierdo, J.L.; Montoya, J.F. [Universidad Nacional de Colombia, Campus Medellín, Departamento de Física, Laboratorio de Materiales Cerámicos y Vítreos, A.A. 568 Medellín (Colombia); Mera, J.; Córdoba, C. [Universidad de Nariño, Centro de Materiales Avanzados, Torobajo, Pasto (Colombia); Gómez, A. [Universidad Nacional de Colombia, Campus Medellín, Facultad de Minas, Laboratorio de caracterización de materiales, A.A. 568 Medellín (Colombia); Paucar, C. [Universidad Nacional de Colombia, Campus Medellín, Departamento de Física, Laboratorio de Materiales Cerámicos y Vítreos, A.A. 568 Medellín (Colombia); Morán, O., E-mail: omoranc@unal.edu.co [Universidad Nacional de Colombia, Campus Medellín, Departamento de Física, Laboratorio de Materiales Cerámicos y Vítreos, A.A. 568 Medellín (Colombia)

2014-06-01

Polycrystalline YBaCo{sub 4}O{sub 7+δ} samples were obtained through a standard solid state reaction, and their structural, morphological, electrical, and magnetic properties are carefully studied. The X-ray powder diffraction (XRD) patterns showed reflections of a pure hexagonal structure (space group P6{sub 3}mc) with lattice parameters being very close to those reported in the literature. Although XRD analysis showed that the main phase present is 114, the presence of secondary phases could not be ruled out based solely on the XRD characterization. Indeed, sensitive SQUID magnetic measurements showed that the samples were affected by very small quantities of the 112 phase (YBaCo{sub 2}O{sub 5.5}), which typically manifests itself through a conspicuous increase in the magnetization at∼300 K. The results achieved corroborated the predictions concerning the difficulty of stabilizing the 114 phase when synthesized via the standard solid-state reaction. With this in mind, we next attempted to obtain the compound with improved phase purity. In so doing, the YBaCo{sub 4}O{sub 7+δ} compound was synthesized through a wet chemistry method based on a citrates route. The XRD patterns recorded for these samples revealed well-defined peaks corresponding to a pure hexagonal structure. More interestingly, SQUID measurements show no sign of features in the M(T) curve at temperatures as low as∼80 K. This result was consistent with the magnetic behavior observed in YBaCo{sub 4}O{sub 7+δ} single-crystals. At temperatures below∼80 K, a clear feature was observed which seemed to correlate with a transition into an antiferromagnetic state. Isothermal magnetization recorded at 70 K showed that field-induced effects manifested themselves through the appearance of a ferromagnetic-like component. This ferromagnetic component may arise from spin canting of the underlying antiferromagnetic state or through field-induced structural transition (at least at local scale). Although a

Synthesis of some new substituted quinazolin-4-3H-ones as potent anticonvulsant agents

International Nuclear Information System (INIS)

Garg, N.; Chandra, T.; Lata, K.K.

2009-01-01

A new series of 3-(4-(2-(6,8-dibromo-3 (substituted phenyl)-4-oxo-3, 4-dihydroquinazolin-2-yl)methyl) hydrazinyl)thiazol-2-yl)-2-phenylthiazolidin-4-ones were synthesized and their structures were elucidated on the basis of elemental analyses and spectroscopic studies (IR, 1H-NMR). All the synthesized compounds 1-32 were screened for their anticonvulsant activity at a dose of 30 mg/kg. The compound 31 was found to be the most potent compound of this series showing 90% protection against MES. (author)

Synthesis, characterization and pharmacological evaluation of different 1,3,4-oxadiazole and acetamide derivatives of ethyl nipecotate

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Khadija Nafeesa

2017-12-01

Full Text Available A new series of N-substituted derivatives of 2-[(5-{1-[(4-chlorophenylsulfonyl]-3-piperidinyl}-1,3,4-oxadiazol-2-ylsulfanyl]acetamide (6a-w has been designed and synthesized with multifunctional moieties. The synthesized compounds were evaluated for their antibacterial and anti-enzymatic potential supported by % hemolytic activity. The synthesized compound 5-(1-(4-chlorophenylsulfonyl-3-piperidinyl-1,3,4-oxadiazole-2-thiol (3 was stirred with synthesized electrophiles as N-aryl/alkyl/aralkyl-2-bromoacetamide (5a-w in an aprotic solvent under basic conditions to acquire the target molecules, 6a-w. The spectral analytical techniques of IR, EI-MS, 1H NMR and 13C-NMR were utilized for structural elucidation of synthesized molecules. The antibacterial screening against certain bacterial strains of gram-negative and gram-positive bacteria rendered compound 6i as good inhibitor of gram-negative bacterial strains. The enzyme inhibition revealed low potential against lipoxygenase (LOX enzyme. The hemolytic study provided valuable information about cytotoxic behavior of synthesized molecules. Keywords: 1,3,4-Oxadiazole, Acetamide, Antibacterial activity, Hemolytic activity, Lipoxygenase inhibition

Rhenium (5) and molybdenum (5) complexes with 4',4''(5'')-ditretbutyldibenzo-24-crown-8. Kompleksnye soedineniya reniya (5) i molibdena (5) s 4',4''(5'')-ditretbutildibenzo-24-kraun-8

Energy Technology Data Exchange (ETDEWEB)

Ashurova, N Kh; Yakubov, K G; Basitova, S M; Tashmukhamedova, A K; Sajfullina, N Zh [Tadzhikskij Gosudarstvennyj Univ., Dushanbe (USSR)

1989-10-01

Rhenium and molybdenum complexes in +5 oxidation degree with 4',4''(5'')-ditretbutyldibenzo-24-crown-8 (L) are synthesized with 75-95 % yield. Composition and structure of compounds produced are investigated using element analysis, conductometry, IR spectroscopy, thermogravimetry methods. Oxidation degree of complexer metal is determined. It is ascertained that the compound composition corresponds to the MOLX{sub 3} formula, where M-Re, Mo; X-Cl{sup -}, Br{sup -}.

SYNTHESIS, CHARACTERIZATION AND ANTIOXIDANT ACTIVITY OF 7-HYDROXY-3',4'-DIMETHOXYFLAVONE

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Elfi Susanti VH

2012-03-01

Full Text Available Synthesis of flavones and their derivatives has attracted considerable attention due to their significant pharmaceutical effects. 7-hydroxy-3',4'-dimethoxyflavone has been synthesized and its antioxidant activity has been investigated. Flavone was synthesized by oxidative cyclization of chalcone. 2',4'-dihydroxy-3,4-dimethoxychalcone was prepared by Claisen-Schmidt condensation of 2,4-dihydroxyacetophenones with 3,4-dimethoxybenzaldehydes in the presence of aqueous solution of sodium hydroxide and ethanol at room temperature. Oxidative cyclization of 2',4'-dihydroxy-3,4-dimethoxychalcone was done by using I2 catalyst in DMSO to form 7-hydroxy-3',4'-dimethoxyflavone. The synthesized compounds were characterized by means of their UV-Vis, IR, 1H-NMR and 13C-NMR spectral data. The compound was tested for their antioxidant activities by DPPH method.

Synthesis, physical-chemical properties of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acid esters

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V. M. Odyntsova

2017-04-01

Full Text Available The nitrogen-containing heterocyclic systems from the class of 1,2,4-triazole derivatives, which exhibit wide range of actions, occupy special place among the variety of heterocyclic compounds. Derived biologically active substances are actively introduced into practice as new original and effective drugs. We were interested in esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids, which exhibit high biological activity and can be intermediates for the synthesis of amides, hydrazides, ylidenderivatives of corresponding acids. The aim of this work is the synthesis of new esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids and the establishment of their physical-chemical properties. Materials and methods. Melting point was determined by open capillary method on the device OptiMelt MPA100. The elemental composition of the synthesized compounds was determined on the universal analyzer ElementarVario ЕL cube (CHNS (standard – sulfanilamide. 1H NMR spectra were recorded on spectrometer Varian Mercury VX-200 (1H, 200 MHz in the solvent dimethyl sulfoxide-d6 (tetramethylsilane internal standard and decoded using a program ADVASP(tm Analyzer program (Umatek International Inc.. Chromato-mass-spectral studies were performed on hazarding chromatograph Agilent 1260 Infinity HPLC equipped with mass spectrometer Agilent 6120 (ionization electro-spray (ESI. The results and discussion. Synthesis of 11 new compounds, namely esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids was carried out by two methods. According to the A method the alkylation of previously synthesized 3-(adamantan-1-yl-1H-1,2,4-triazole-5-thiol was performed with the use of corresponding methyl ester of 2-chloroacetic acid and the presence of equivalent amount of sodium hydroxide. The B method involves the etherification of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acid with the use of methyl, ethyl, i

Synthesis of 3-Methyl-1-morpholin-4-ylmethyl-2,6-diphenylpiperidin-4-one

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Bathey R. Venkatraman

2009-09-01

Full Text Available This paper describes the synthesis of 3-methyl-1-morpholin-4-ylmethyl-2,6-diphenylpiperidin-4-one from 3-methyl-2,6-diphenylpiperidin-4-one. The synthesized compound was characterized by FT-IR, 1H NMR, EI-MS and elemental analysis.

Water linked 3D coordination polymers: Syntheses, structures and applications

Science.gov (United States)

Singh, Suryabhan; Bhim, Anupam

2016-12-01

Three new coordination polymers (CPs) based on Cd and Pb, [Cd(OBA)(μ-H2O)(H2O)]n1, [Pb(OBA)(μ-H2O)]n2 [where OBA=4,4'-Oxybis(benzoate)] and [Pb(SDBA)(H2O)]n.1/4DMF 3 (SDBA=4,4'-Sulfonyldibenzoate), have been synthesized and characterized. The single crystal structural studies reveal that CPs 1 and 2 have three dimensional structure. A water molecule bridges two metal centres which appears to the responsible for the dimensionality increase from 2D to 3D. Compound 3 has a supramolecular 3D structure involving water molecule and hydrogen bonds. A structural transformation is observed when 3 was heated at 100 °C or kept in methanol, forming [Pb(SDBA)]n4. Compound 4 is used as supporting matrix for palladium nanoparticles, PdNPs@4. The PdNPs@4 exhibits good catalytic activity toward the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the presence of NaBH4 at room temperature. Luminescence studies revealed that all CPs could be an effective sensor for nitroaromatic explosives.

Synthesis, physical-chemical properties of 2-((4-R-5-(thiophene-2-ylmethyl-4H-1,2,4-triazole-3-ylthioacetohydrazides

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O. A. Suhak

2017-04-01

Full Text Available Aim. Analysis of the scientific literature over the past decade has shown that large synthetic possibilities towards creating new and effective drug substances have heterocyclic compounds, in particular the derivatives of 1,2,4-triazole. 1,2,4-Triazole is a structural fragment of many synthetic drugs. The special interest cause ylidene hydrazides of 2-(5-R-1,2,4-triazole-3-ylthioacetic acids as potential biologically active compounds, among which highly effective medicines can be found. With the aim of finding new biologically active compounds the derivatives of 2-((4-R-5-(thiophene-2-ylmethyl-4H-1,2,4-triazole-3-ylthioaceticohydrazides have been synthesized, their physical-chemical properties have been studied with the use of modern methods, namely elemental analysis, IR,1H-NMR spectroscopy, and their individuality by HPLC-MS. Materials and methods. N'-R1-еden-2-((4-R-5-(thiophene-2-ylmethyl-4H-1,2,4-triazole-3-ylthioaceticohydrazides were received by adding aromatic (2-BrC6H4, 2,3-(OCH32C6H3, 3,5-(OCH32C6H3, 4-N(CH32C6H4, 3,4-F2C6H3, 2-NO2C6H4,4-NO2C6H4, 4-OHC6H4, 2-OHC6H4, 4-FC6H4, 2-CI-6-FC6H3 or heterocyclic (2-SC4H3, 5-NO2-2-C4H2O aldehyde to an equivalent amount of the appropriate 2-((4-R-5-(thiophene-2-ylmethyl-4H-1,2,4-triazole-3-ylthioaceticohydrazide in the acetic acid medium. The study of physical-chemical properties of obtained compounds was carried out according to the methods outlined in SPU. Chromato-mass-spectral studies were performed on hazarding chromatograph Agilent 1260 Infinity HPLC equipped with mass spectrometer Agilent 6120 with ionization in electro-spray (ESI. Conclusion. This suggests the possibility for further study of biological action of the synthesized compounds. As a result of studies the N'-R1-eden-2-((4-R-5-(thiophene-2-ylmethyl-4H-1,2,4-triazole-3-ylthioaceticohydrazides have been synthesized and their physical-chemical properties have been studied.

Synthesis of novel styryl derivatives from 4-chloro-2-(morpholin-4-yl)-1,3-thiazole-5-carbaldehyde, study of their photophysical properties and TD-DFT computations

International Nuclear Information System (INIS)

Sekar, Nagaiyan; Umape, Prashant G.; Padalkar, Vikas S.; Tayade, Rajratna P.; Ramasami, Ponnadurai

2014-01-01

Novel fluorescent styryl push–pull compounds having electron donating thiazole unit were synthesized by condensing 4-chloro-2-(morpholin-4-yl)-1,3-thiazole-5-carbaldehyde with active methylene compounds via classical Knoevenagel condensation. The synthesized styryl molecules were characterized by spectral analysis. Photophysical properties of these styryl derivatives were analyzed and the effect of change in solvent polarity and viscosity on their absorptive and emissive properties has been investigated. Density functional theory (DFT) and time dependent-density functional theory (TD-DFT) computations have been used to understand the structural, molecular, electronic and photophysical parameters of push–pull dyes. Bakhshiev and Kawski–Chamma–Viallet correlations were used to calculate the ratio of ground to excited state dipole moment of the synthesized novel styryl compounds. -- Highlights: •Novel styryl derivatives are synthesized from thiazole aldehyde. •Photophysical properties of styryl derivatives were evaluated and supported by TD-DFT computations. •Experimental photophysical results are in good agreement with the theoretical results obtained by TD-DFT computations. •Compounds show fluorescence in solid state as well as in solvents of different polarities

Site preferences of actinide cations in [NZP] compounds

Science.gov (United States)

Hawkins, H. T.; Spearing, D. R.; Smith, D. M.; Hampel, F. G.; Veirs, D. K.; Scheetz, B. E.

2000-07-01

Compounds adopting the sodium dizirconium tris(phosphate) (NaZr2(PO4)3) structure type belong to the [NZP] structural family of compounds. [NZP] compounds possess desirable properties that would permit their application as hosts for the actinides. These properties include compositional flexibility (i.e., three structural sites that can accommodate a variety of different cations), high thermal stability, negligible thermal expansion, and resistance to radiation damage. Experimental data indicate that [NZP] compounds resist dissolution and release of constituents over a wide range of experimental conditions. Moreover, [NZP] compounds may be synthesized by both conventional and novel methods and may be heat treated or sintered at modest temperatures (800 °C-1350 °C) in open or restricted systems.

Rhenium (5) and molybdenum (5) complexes with 4',4''(5'')-ditretbutyldibenzo-24-crown-8

International Nuclear Information System (INIS)

Ashurova, N.Kh.; Yakubov, K.G.; Basitova, S.M.; Tashmukhamedova, A.K.; Sajfullina, N.Zh.

1989-01-01

Rhenium and molybdenum complexes in +5 oxidation degree with 4',4''(5'')-ditretbutyldibenzo-24-crown-8 (L) are synthesized with 75-95 % yield. Composition and structure of compounds produced are investigated using element analysis, conductometry, IR spectroscopy, thermogravimetry methods. Oxidation degree of complexer metal is determined. It is ascertained that the compound composition corresponds to the MOLX 3 formula, where M-Re, Mo; X-Cl - , Br -

Design, Synthesis, Antibacterial and Antifungal Activity of Novel 2-[(E-2-aryl-1-ethenyl]-3-(2-sulfanyl-1H-benzo[d]imidazole-5-yl-3,4- dihydro-4-quinolinones

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Anisetti Ravinder Nath

2012-01-01

Full Text Available The novel 2-[(E-2-aryl-1-ethenyl]-3-(2-sulfanyl-1H-benzo[d]imidazole-5-yl-3,4- dihydro-4-quinolinones (4a-j analogs were synthesized by Knoevenagel condensation of a solution of 2-methyl-3-(2-sulfanyl-1H-benzo[d]imidazole-5-yl-3,4-dihydro-4-quinazolinone (3 with aromatic aldehyde in presence of catalytic amount of piperidine. Compounds (4a-j showed significant biological activity against all the standard strains. All the synthesized compounds were characterized on the basis of their IR, 1H NMR, MASS spectroscopic data and elemental analyses. All the compounds have been tested for antimicrobial and antifungal activity by the cup-plate method.

Synthesis, crystal structures, fluorescence and xanthine oxidase inhibitory activity of pyrazole-based 1,3,4-oxadiazole derivatives

Science.gov (United States)

Qi, De-Qiang; Yu, Chuan-Ming; You, Jin-Zong; Yang, Guang-Hui; Wang, Xue-Jie; Zhang, Yi-Ping

2015-11-01

A series of pyrazole-based 1,3,4-oxadiazole derivatives were rationally designed and synthesized in good yields by following a convenient route. All the newly synthesized molecules were fully characterized by IR, 1H NMR and elemental analysis. Eight compounds were structurally determined by single crystal X-ray diffraction analysis. The fluorescence properties of all the compounds were investigated in dimethyl sulfoxide media. In addition, these newly synthesized compounds were evaluated for in vitro inhibitory activity against commercial enzyme xanthine oxidase (XO) by measuring the formation of uric acid from xanthine. Among the compounds synthesized and tested, 3d and 3e were found to be moderate inhibitory activity against commercial XO with IC50 = 72.4 μM and 75.6 μM. The studies gave a new insight in further optimization of pyrazole-based 1,3,4-oxadiazole derivatives with excellent fluorescence properties and XO inhibitory activity.

Crystal structure and electrical conduction of the new organic-inorganic compound (CH2)2(NH3)2CdI4

Science.gov (United States)

Zhang, Liuqi; Wang, Jilin; Han, Feifei; Mo, Shuyi; Long, Fei; Gao, Yihua

2018-03-01

The new organic-inorganic compound (CH2)2(NH3)2CdI4 was prepared by slow evaporation method using a mixture solution of CdI2 and ethylenediamine iodide (EDAI) in the γ-butyrolactone (GBL). The synthesized compound was further characterized by single crystal diffraction, Infrared (IR) and Raman spectroscopy, energy dispersive spectrometer (EDS), X-Ray photoelectron spectroscopy (XPS) and thermogravimetric analysis. The relaxation behavior and conductivity mechanism of (CH2)2(NH3)2CdI4 was studied by the electrical impedance spectroscopy. The results indicated that (CH2)2(NH3)2CdI4 had a monoclinic structure with space group P21/c at room temperature. The complex impedance plotted as semicircle arcs and the proposed electrical equivalent circuit was to interpret the impedance behavior at different temperatures. The electrical equivalent circuit was made of a parallel combination of resistance (R) and fractal capacitance (CPE). Furthermore, the alternating current conductivity of the sample obeyed the Jonscher's law: σf =σdc + Afs and the conduction could be attributed to the correlated barrier hopping (CBH) model.

Stereocontrolled dopamine receptor binding and subtype selectivity of clebopride analogues synthesized from aspartic acid.

Science.gov (United States)

Einsiedel, Jürgen; Weber, Klaus; Thomas, Christoph; Lehmann, Thomas; Hübner, Harald; Gmeiner, Peter

2003-10-06

Employing the achiral 4-aminopiperidine derivative clebopride as a lead compound, chiral analogues were developed displaying dopamine receptor binding profiles that proved to be strongly dependent on the stereochemistry. Compared to the D1 receptor, the test compounds showed high selectivity for the D2-like subtypes including D2(long), D2(short), D3 and D4. The highest D4 and D3 affinities were observed for the cis-3-amino-4-methylpyrrolidines 3e and the enantiomer ent3e resulting in K(i) values of 0.23 and 1.8 nM, respectively. The benzamides of type 3 and 5 were synthesized in enantiopure form starting from (S)-aspartic acid and its unnatural optical antipode.

Synthesis, antimicrobial and cytotoxic activities of 5-benzylidene-2-[(pyridine-4-ylmethylenehydrazono]-thiazolidin-4-one and 2-[(pyridine-4-ylmethylene hydrazono]-thiazolidin-4-one derivatives

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Danniel Delmondes Feitoza

2012-01-01

Full Text Available A new series of 5-benzylidene-2-[(pyridine-4-ylmethylenehydrazono]-thiazolidin-4-ones 4a-l have been synthesized. These compounds were designed by a molecular hybridization approach. 2-[(Pyridine-4-ylmethylenehydrazono]-thiazolidin-4-ones 3a-d were also obtained and used as intermediates to give the target compounds. The in vitro antimicrobial and cytotoxic activities were evaluated for both series. The intermediate 3b showed considerable antibiotic activity against B. subtilis and C. albicans. In the cytotoxic activity compounds 3b (IC50= 4.25 ± 0.36 µg/mL and 4l (IC50= 1.38 ± 0.04 µg/mL were effective for inhibition of human erythromyeloblastoid leukemia (K-562 and human lung carcinoma (NCI-H292 cell lines, respectively.

Studying the interaction between three synthesized heterocyclic sulfonamide compounds with hemoglobin by spectroscopy and molecular modeling techniques.

Science.gov (United States)

Naeeminejad, Samane; Assaran Darban, Reza; Beigoli, Sima; Saberi, Mohammad Reza; Chamani, Jamshidkhan

2017-11-01

The interaction between synthesized heterocyclic benzene sulfonamide compounds, N-(7-benzyl-56-biphenyl-2m-tolyl-7H-pyrrolo[23-d]pyrimidine-4-yl)-benzene sulfonamide (HBS 1 ), N-(7-benzyl-56-biphenyl-2-m-tolyl-7H-pyrrolo[23-d] pyrimidine-4-yl)-4-methyl- benzene sulfonamide (HBS 2 ), and N-(7-benzyl-56-biphenyl-2-m-tolyl-7H-pyrrolo[23-d]pyrimidine-4-yl)-4-chloro-benzene sulfonamide (HBS 3 ) with Hb was studied by fluorescence quenching, zeta potentional, circular dichroism, and molecular modeling techniques. The fluorescence spectroscopy experiments were performed in order to study the conformational changes, possibly due to a discrete reorganization of Trp residues during binding between HBS derivatives and Hb. The variation of the K SV value suggested that hydrophobic and electrostatic interactions were the predominant intermolecular forces stabilizing the complex. The K SV1 ans K SV2 values of HBS derivatives with Hb are .6 × 10 13 and 3 × 10 13  M -1 for Hb-HBS 1 , 1 × 10 13 and 4 × 10 13  M -1 for Hb-HBS 2 , .9 × 10 13 , and 6 × 10 13  M -1 for Hb-HBS 3 , respectively. The molecular distances between Hb and HBS derivatives in binary and ternary systems were estimated according to Förster's theory of dipole-dipole non-radiation energy transfer. The quantitative analysis data of circular dichroism spectra demonstrated that the binding of the three HBS derivatives to Hb induced conformational changes in Hb. Changes in the zeta potential of the Hb-HBS derivatives complexes demonstrated a hydrophobic adsorption of the anionic ligand onto the surface of Hb as well as both electrostatic and hydrophobic adsorption in the case of the complex. The modeling data thus confirmed the experimental results. This study is expected to provide important insight into the interaction of Hb with three HBS derivatives to use in various toxicological and therapeutic processes.

Design, Synthesis and the Biological Evaluation of New 1,3-Thiazolidine-4-ones Based on the 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one Scaffold

Directory of Open Access Journals (Sweden)

Maria Apotrosoaei

2014-09-01

Full Text Available New thiazolidine-4-one derivatives based on the 4-aminophenazone (4-amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one scaffold have been synthesized as potential anti-inflammatory drugs. The pyrazoline derivatives are known especially for their antipyretic, analgesic and anti-inflammatory effects, but recently there were synthesized new compounds with important antioxidant, antiproliferative, anticancer and antidiabetic activities. The beneficial effects of these compounds are explained by nonselective inhibition of cyclooxygenase izoenzymes, but also by their potential scavenging ability for reactive oxygen and nitrogen species. The structure of the new compounds was proved using spectroscopic methods (FR-IR, 1H-NMR, 13C-NMR, MS. The in vitro antioxidant potential of the synthesized compounds was evaluated according to the ferric reducing antioxidant power, phosphomolydenum reducing antioxidant power, DPPH and ABTS radical scavenging assays. The chemical modulation of 4-aminophenazone (6 through linkage to thiazolidine-propanoic acid derivatives 5a–l led to improved antioxidant potential, all derivatives 7a–l being more active than phenazone. The most active compounds are the derivatives 7e, and 7k, which showed the higher antioxidant effect depending on the antioxidant assay considered.

Vibrational spectroscopic and dielectric properties investigations of phase transitions in KMgPO4 compound

Science.gov (United States)

Miladi, L.; Oueslati, A.; Guidara, K.

2017-11-01

The potassium orthophosphate KMgPO4 with a β-tridymite structure was synthesized via solid-state reaction. X-ray diffraction study confirms the formation of a single phase material which crystallizes at room temperature in monoclinic system. This compound has been investigated by vibrational spectroscopy in the temperature range573-723 K. Thermal analysis shows that this composition undergoes two phase transitions at T1=633Kand T2=693 K.The evolution of Raman line ν and half -width Δν versus temperature introduces huge changes which are associated with the phase transitions originating from the reorientation of the PO4 tetrahedron. Besides, an analysis of the dielectric constants ε‧ and ε″versus temperature at several frequencies shows a distribution of relaxation times. This relaxation is probably due to the change in dynamical state of the K+ cation. The ac conductivity behavior can be understood in terms of the motions of K+ cations along the tunnels which are formed by six-membered rings of MgO4 and PO4 tetrahedron linked by common vertices. The activation energies values obtained from the thermal evolution of the conductivity are: Ea1=0.52 eV (T693 K).

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

International Nuclear Information System (INIS)

Qian, Cheng; Kong, Fang; Mao, Jiang-Gao

2016-01-01

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 (1), Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 ·0.5H 2 O (2) and Cu 2 (2,2-bipy) 2 V 5 O 12 (SeO 3 ) 2 (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 } 2 dimeric cluster composed of two {Ni(2,2-bipy) 2 } 2+ moieties connected by the {V 4 O 8 (SeO 3 ) 4 } 4- cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 } n chain in which the {Cu 2 (2,2-bipy) 2 } 4+ moieties are bridged by the {V 4 O 8 (SeO 3 ) 4 } 4− clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {V IV V V 4 Se IV 2 O 18 } n 4− and {Cu(2,2-bipy)} 2+ complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V 4 O 8 (SeO 3 ) 4 } 4− cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties. - Graphical abstract: We got three new vanadium selenites with organically linked copper/nickel complex, namely, Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 (1), Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 ·0.5H 2 O (2) and Cu 2 (2,2-bipy) 2 V 5 O 12 (SeO 3 ) 2 (3) by hydrothermally syntheses. They display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. Display Omitted - Highlights: • Three new compounds display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. • The Tetranuclear {V 4 O 8 (SeO 3 ) 4 } 4− cluster and the vanadate {V 5 O 17 } n 2D layer are observed firstly. • Optical Properties and Magnetic Properties of three compounds are reported.

Syntheses, structures, photoluminescence and photocatalysis of 2D layered lanthanide-carboxylates with 2, 2′-dithiodibenzoic acid

Energy Technology Data Exchange (ETDEWEB)

Ding, Ling; Zhong, Jie-Cen; Qiu, Xing-Tai; Sun, Yan-Qiong, E-mail: sunyq@fzu.edu.cn; Chen, Yi-Ping

2017-02-15

Two series of lanthanide-carboxylates, [Ln(2,2′-dtba)(2,2′-Hdtba)(EtOH)]{sub n} (I:Ln=Eu(1a), Dy(1b)) and [Ln(2,2′-dtba)(2,2′-Hdtba)(4,4′-bpy){sub 0.5}]{sub n} (II:Ln=Eu(2a), Dy(2b), Tb(2c) 2,2′-H{sub 2}dtba=2,2′-dithiodibenzoic acid, 4,4′-bpy=4,4′-bipyridine) have been synthesized under hydrothermal conditions. Interestingly, the H{sub 2}dtba organic ligand was generated by in situ S–S reaction of 2-mercaptobenzoic acid. Compounds I and II possess different 2D layered structures based on similar 1D [Ln(2,2′-dtba)]{sup +} chains. Photoluminescence studies reveal that compounds I and II exhibit strong lanthanide characteristic emission bands. Remarkably, Compounds 1b and 2a both exhibit good photocatalytic activity for degradation of Rhodamine-B (Rh-B) under the simulated sunlight irradiation. - Graphical abstract: Two series of lanthanide-carboxylates have been in situ synthesized under hydrothermal conditions. The lanthanide-carboxylates exhibit strong lanthanide characteristic emission bands and good photocatalytic activity for degradation of Rhodamine-B. - Highlights: • 2D layered lanthanide-carboxylates with 2,2′-dithiodibenzoic acid. • In situ S–S reaction of 2-mercaptobenzoic acid under hydrothermal condition. • The Emission spectra of I and II exhibit the characteristic transition of lanthanide ions. • Compounds 1b and 2a exhibit good photocatalytic activity for degradation of Rhodamine-B.

Synthesis and investigation of CrB{sub 4}, MnB{sub 4} and new ternary chromium and rhenium manganese borides; Synthese und Untersuchung von CrB{sub 4}, MnB{sub 4} sowie neuen ternaeren Chrom- und Rheniummanganboriden

Energy Technology Data Exchange (ETDEWEB)

Knappschneider, Arno

2014-10-13

In the present work single crystals of the tetraborides of chromium and manganese have been grown and allowed a structure refinement of the compounds. Furthermore the physical characteristics for example hardness, electronic properties and magnetism were been determined. Also the ternary tetraboride phase of chromium and manganese was synthesized and a new ternary rhenium manganese diboride could be obtained.

Synthesis and characterization of some novel 1,2,4-triazoles, 1,3,4-thiadiazoles and Schiff bases incorporating imidazole moiety as potential antimicrobial agents

KAUST Repository

Aouad, Mohamed Reda

2015-05-23

(1,4,5-Triphenylimidazol-2-yl-thio)butyric acid hydrazide (3) was obtained via alkylation of 1,4,5-triphenylimidazol-2- thiol (1) with ethylbromobutyrate, followed by addition of hydrazine hydrate. Treatment of acid hydrazide 3 with carbon disulfide in an ethanolic potassium hydroxide solution gave the intermediate potassium dithiocarbazinate salt, which was cyclized to 4-amino-5-[(1,4,5-triphenylimidazol- -2-yl)thiopropyl]-2H-1,2,4-triazole-3-thione (4) in the presence of hydrazine hydrate. Condensation of compound 3 with alkyl/arylisothiocyanate afforded the corresponding 1-[4-(1,4,5-triphenylimidazol-2-ylthio)butanoyl]-4-alkyl/arylthiosemicarbazides (5-7), which upon refluxing with sodium hydroxide, yielded the corresponding 1,2,4-triazole - -3-thiols 8-10. Under acidic conditions, compounds 4-6 were converted to aminothiadiazoles 11-13. Moreover, the series of Schiff bases 14-18 were synthesized from the condensation of compound 3 with different aromatic aldehydes. The newly synthesized compounds were characterized by IR, 1H NMR, 13C NMR and mass spectral analyses. They were also preliminarily screened for their antimicrobial activity.

THE SYNTHESIS OF RGDF MIMETIC DERIVATIVES BASED ON 4-(ISOINDOLINE-5-YLAMINO-4-OXOBUTYRIC ACID WITH THE ORAL ANTIAGGREGATIVE ACTIVITY

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A. A. Krysko

2015-03-01

Full Text Available Ethyl ethers of N-[4-(isoindoline-5-ylamino-4-oxobutyryl]-D,L-β-substituted-β-alanines were synthesized. Estimation of antiaggregatory activity of the compounds obtained has showed that the compounds possess an oral activity ex vivoin mice  with the use of human rich platelet plasma.

Synthesis, antimicrobial and cytotoxic activities of 5-benzylidene-2-[(pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-one and 2-[(pyridine-4-ylmethylene) hydrazono]-thiazolidin-4-one derivatives

Energy Technology Data Exchange (ETDEWEB)

Feitoza, Danniel Delmondes; Alves, Antonio Jose; Lima, Jose Gildo de, E-mail: jgildolima@gmail.com [Departamento de Ciencias Farmaceuticas, Universidade Federal de Pernambuco, Recife - PE (Brazil); Araujo, Janete Magali; Aguiar, Jaciana Santos; Rodrigues, Maria do Desterro; Silva, Teresinha Goncalves; Nascimento, Silene Carneiro do; Goes, Alexandre Jose da Silva [Departamento de Antibioticos, Universidade Federal de Pernambuco, Recife - PE (Brazil)

2012-07-01

A new series of 5-benzylidene-2-[(pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-ones 4a-l have been synthesized. These compounds were designed by a molecular hybridization approach. 2-[(Pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-ones 3a-d were also obtained and used as intermediates to give the target compounds. The in vitro antimicrobial and cytotoxic activities were evaluated for both series. The intermediate 3b showed considerable antibiotic activity against B. subtilis and C. albicans. In the cytotoxic activity compounds 3b (IC{sub 50} = 4.25 +- 0.36 {mu}g/mL) and 4l (IC{sub 50} = 1.38 +- 0.04 {mu}g/mL) were effective for inhibition of human erythromyeloblastoid leukemia (K-562) and human lung carcinoma (NCI-H292) cell lines, respectively. (author)

Compounds of Fe-Zn bond

International Nuclear Information System (INIS)

Mauro, A.E.; Mancini, M.N.G.

1981-01-01

The compounds of the type L 1 L 2 ZnFe(CO) 4 , not yet reported, are synthesized and studied by infrared spectroscopy. The data are interpreted based on a monomeric structure with a local C sub(3v) symmetry around the iron atom. L 1 = methylamine (Mea), dimethylamine (diMea), trimethylamine (triMea) L 2 = ethylenediamine (en), N-methylethylenediamine (N,Meen), N,N-dimethylenthylenediamines, (s-diMeen). (Author) [pt

Synthesis and Biological Activity of 3-(2-Furanyl-6-Aryl-1,2,4-Triazolo[3,4-b]-1,3,4 –Thiadiazoles

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Zi-Yi Zhang

2002-08-01

Full Text Available 3-(2-Furanyl-4-amino-5-mercapto-1,2,4-triazole (1 was prepared from 2-furoic acid through a multi-step reaction sequence. Compound 1 reacted with aromatic acids in the presence of phosphorus oxychloride to give 3-(2-furanyl-6-aryl-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles (2. The structures of all the newly synthesized compounds have been confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and mass spectra. The bioassay indicated most of the title compounds possess significant growth promoting effects on mung bean radicles.

Removal of emulsified and dissolved traces of organic compounds from industrial wastewaters using nature and synthesized (Na A and Nam) zeolites

International Nuclear Information System (INIS)

Modirshahla, N.; Tabatabaii, S.

2004-01-01

The main object of this study was to compare the natural and synthetic (Na A and Nam) zeolites as absorbents in removing emulsified and dissolved traces of organic compounds, which appear in the wastewater of power plants, refinery and petrochemical complexes. The specific objections of the work was: a) to select the best species that have the highest amount of absorption; b) to measure the rate of absorption of traces organic compounds and emulsions on the natural and synthesized zeolites; c) to establish the absorption isotherms for the organics and emulsions with selected samples; d) to select readily available regenerants, and e ) to examine the ph dependence of the process and to establish a simple and practical method to detect and to measure the pollution after the treatment process. The BOD and COD of the treated and feed waters were compared

Synthesis and Antimicrobial Activity of N-[2-(aryl/substituted aryl)-4-oxo-1,3-thiazolidin-3-yl]pyridine-4-carboxamide

International Nuclear Information System (INIS)

Thomas, Asha B.; Nanda, Rabindra K.; Kothapalli, Lata P.; Deshpande, Avinash D.

2011-01-01

A series of isonicotinyl hydrazones and their 4-thiazolidinones have been synthesized by condensation of isonicotinic acid hydrazide with various aromatic aldehydes to yield Schiff's bases, followed by the cyclocondensation of Schiff's bases with 2-mercaptoacetic acid to yield their 4-thiazolidinones. The synthesized compounds have been characterized by their elemental, analytical and spectral studies. All these compounds were evaluated for their in vitro antimicrobial activity against a spectrum of non-resistant and resistant microbial organisms. These studies proved that compounds 5e,i against B. subtilis; 5e,f,h against B. anthracis; 5g,i against S. aureus showed good activity at lower concentrations. Compounds 5d-5i displayed significant activity against resistant strain of K. pneumonia with minimum inhibitory potency in the concentration range of 2-16 ug/ml

Synthesis and studies of some organometallic compounds of uranium IV

International Nuclear Information System (INIS)

Marquet-Ellis, Hubert; Folcher, Gerard.

1975-06-01

The organometallic compounds of uranium IV have been well known for a long-time but some difficulties in the synthese subsist. The procedures and the apparatus allowing to obtain these compounds with good yields are described. The cyclopenta dienyl compounds U(C 5 H 5 ) 3 Cl, U(C 5 H 5 ) 4 are prepared by reaction of UCl 4 with Na(C 5 H 5 ) in tetrahydrofurane. The cyclooctatetraene compound U(C 8 H 8 ) 2 ''Uranocene'' is obtained by reaction of K 2 (C 8 H 8 ) on UCl 4 in tetrahydrofurane. The NMR spectrum of the solution during the reaction shows the appearance of the product. These compounds have been identified by chemical analysis and X rays. The visible spectra of U(C 5 H 5 ) 2 Cl and U(C 8 H 8 ) 2 in gaseous phase have been obtained [fr

Syntheses, characterizations and crystal structures of three new organically templated or organically bonded zinc selenates

International Nuclear Information System (INIS)

Feng Meiling; Mao Jianggao; Song Junling

2004-01-01

Three new organically templated or organically bonded zinc selenates, namely, {H 2 bipy}Zn(SeO 4 ) 2 (H 2 O) 2 1 (bipy=4,4'-bipyridine), {H 2 pip}{Zn(SeO 4 ) 2 (H 2 O) 4 }·2H 2 O 2 (pip=piprazine), and Zn(SeO 4 )(phen)(H 2 O) 2 3 (phen=1,10-phenanthroline) have been synthesized by hydrothermal reactions. The structure of compound 1 features a 1D chain composed of [Zn(SeO 4 ) 2 (H 2 O) 2 ] 2- anions. Compound 2 has a 2D layer structure built from {Zn(SeO 4 ) 2 (H 2 O) 4 } 2- anions that are cross-linked by doubly protonated piperazine cations via N-H···O hydrogen bonds. The structure of compound 3 contains a 1D chain of Zn(SeO 4 )(phen)(H 2 O) 2 , such chains are further interlinked by hydrogen bonds and π···π interactions to form a layer. The different roles the templates played have also been discussed

Synthesis and Antibacterial Evaluation of Novel Heterocyclic Compounds Containing a Sulfonamido Moiety

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Eman A. El-Bordany

2013-01-01

Full Text Available Aiming for the synthesis of new heterocyclic compounds containing a sulfonamido moiety suitable for use as antibacterial agents, the precursor ethyl {[4-N-(4,6-dimethylpyrimidin-2-ylsulfamoyl]phenylazo}cyanoacetate was reacted with a variety of active methylene compounds producing pyran, pyridine and pyridazine derivatives. Also, the reactivity of the precursor hydrazone towards hydrazine derivatives to give pyrazole and oxazole derivatives was studied. On the other hand, treatment of the same precursor with urea, thiourea and/or guanidine hydrochloride furnished pyrimidine and thiazine derivatives, respectively. The newly synthesized compounds were tested for antibacterial activity, whereby eight compounds were found to have high activities.

Synthesis of morpholine derivatives and Bunte's salt as compounds of potential radioprotective activity

Energy Technology Data Exchange (ETDEWEB)

Strzelczyk, M.; Kucharski, A. (Wojskowa Akademia Medyczna, Lodz (Poland))

1980-01-01

The purpose of the present study was to obtain several compounds possessing radioprotective activity. The syntheses yielded seven undescribed compounds i.e.: benzyl ester of the N-morpholinecarbathionothioglicol acid, ester bis S-(morpholine-4-thiocarbonyl)-2-thioethyl, morpholine salt of the N-morpholinecarbothionothiolic acid, sodium and potassium salt of S-morpholine-4-carbonyl, methylthiosulfate, sodium and potassium salt of beta-hydroxyethyl thiosulfate. Moreover, with the aid of other methods following compounds were synthetized: beta-S-(morpholine-4-thiocarbonyl) ethyl thiopropioniane, amide of the S-(morpholine-4-thiocarbonyl)-thioglicol acid, acid S-(morpholine-4-thiocarbonyl)-thioglicol acid, sodium salt of the S-(morpholine-4-thiocarbonyl)-thioglicol acid. The structure of these compounds was confirmed using elementary and spectral analysis.

Synthesis and Biological Activity of 3-Chloro-1-(4-perimidine methylcarbonylamino-4-phenyl-azetidin-2-one

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Dinesh R. Panchasara

2009-01-01

Full Text Available Perimidine-1-acetic acid hydrazide (1 undergoes facile condensation with aromatic aldehydes to afford the corresponding azomethine (i.e. Schiff base derivatives (2a-h in good yield. Cyclocondensation of compounds (2a-h with chloro acetyl chloride affords 3-chloro-1-(4-perimidine methylcarbonylamino-4-phenyl-azetidin-2-ones (3a-h. The structures of these compounds were established on the basis of analytical and spectral data. The newly synthesized compounds were evaluated for their antibacterial and antifungal activities.

Actoprotective properties of 7'-((3-thio-4-methyl-4H-1,2,4-triazole-5-ylmethyltheophylline derivatives

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A. S. Gotsulya

2016-06-01

Full Text Available The aim of this work was the study of actoprotective activity of compounds, which combine sintons of 1,2,4-triazole-3-thiol and theophylline. Materials and methods. The first time synthesized 7'-((3-thio-4-phenyl-4H-1,2,4-triazole-5-ylmethyltheophylline derivatives have been used for the research. The systemic toxicity and the acute toxicity of the studied compounds have been performed by the rapid method of Prozorovskiy to determine the optimal conditions for dispensing substances. Experiments have been conducted on a group of white nonlinear rats, 159–221 g weight. During the study of actoprotective activity the method of forced immersion in water with a load of 10% by weight of the rats has been used. The substances were administered at a dose 1/10 of LD50, and the reference drug «Riboxin» at a dose of 100 mg/kg. The swim time was recorded in seconds. The control group of animals was used for comparison; these animals received saline solution intraperitoneally 20 minutes before immersion. The obtained results were statistically processed using the standard software package of Microsoft Office 2007 and «STATISTICA@ for Windows 6.0». Results. According to the results of conducted researches it has been established that the most active compound among the studied was 7'-((5-(2-hydroxyethylthio-4-phenyl-4H-1,2,4-triazole-3-ylmethyltheophylline, which increased the duration of swimming by 14.31% comparing to control group, whereas the reference drug increased it by 20.57%. It has been established that 2-((5-((theophylline-7'-ylmethyl-4-phenyl-4H-1,2,4-triazol-3-ylthio-N'-(3,4-difluorobenzylideneacetohydrazide also increases the duration of swimming. Conclusion. The study of actoprotective activity of 13 first time synthesized compounds has been conducted. 7'-((5-(2-Hydroxyethylthio-4-phenyl-4H-1,2,4-triazole-3-ylmethyltheophylline has been detected as the most active compound among the studied ones.

Essential oils-oriented fenvalerate analogues: syntheses, characterization and biological evaluation

International Nuclear Information System (INIS)

Su, H.; Li, H.

2016-01-01

A series of essential oils oriented ester derivatives have been designed, synthesized and characterized based on the skeleton of fenvalerate. The preliminary bioassay results indicated that some of the newly synthesized compounds showed better insecticidal activities against Pyrausta nubilalis and Heliothis armigera than that of the control trans-prallethrin chloride. (author)

Structure Modification of an Active Azo-Compound as a Route to New Antimicrobial Compounds

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Simona Concilio

2017-05-01

Full Text Available Some novel (phenyl-diazenylphenols 3a–g were designed and synthesized to be evaluated for their antimicrobial activity. A previously synthesized molecule, active against bacteria and fungi, was used as lead for modifications and optimization of the structure, by introduction/removal or displacement of hydroxyl groups on the azobenzene rings. The aim of this work was to evaluate the consequent changes of the antimicrobial activity and to validate the hypothesis that, for these compounds, a plausible mechanism could involve an interaction with protein receptors, rather than an interaction with membrane. All newly synthesized compounds were analyzed by 1H-NMR, DSC thermal analysis and UV-Vis spectroscopy. The in vitro minimal inhibitory concentrations (MIC of each compound was determined against Gram-positive and Gram-negative bacteria and Candida albicans. Compounds 3b and 3g showed the highest activity against S. aureus and C. albicans, with remarkable MIC values of 10 µg/mL and 3 µg/mL, respectively. Structure-activity relationship studies were capable to rationalize the effect of different substitutions on the phenyl ring of the azobenzene on antimicrobial activity.

Enhancement of the electrochemical performance in LiFePO4 cathode materials synthesized by using the sol-gel method

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Kyong-Soo Hong

2010-11-01

Full Text Available LiFePO4 powders were synthesized by using the sol-gel and the solid-state reaction methods. The chemical states of Fe ions were studied by using XPS, and their electrochemical properties according to the oxidation states of Fe ions were compared. The average oxidation state of Fe ions in LiFePO4 powders synthesized by using the solid-state reaction method was found to be Fe3+, on the other hand, that of Fe ions synthesized by using the sol-gel method was found to be Fe2+. The obtained discharge capacities were 50 mAh/g and 120 mAh/g at a rate 0.1 C in LiFePO4 synthesized by using the solid-state reaction and sol-gel methods, respectively. Relatively a good cycling stability was observed in sol-gel prepared powder.

The thermal expansion of a highly crystalline hexagonal BC2N compound synthesized under high temperature and pressure

International Nuclear Information System (INIS)

Wu Qinghua; Liu Zhongyuan; Hu Qianku; Li Hui; He Julong; Yu Dongli; Li Dongchun; Tian Yongjun

2006-01-01

The thermal expansion has been investigated for a highly crystalline hexagonal BC 2 N compound synthesized by the compression of a turbostratic B-C-N precursor with iron catalyst at the high temperature of 1500 deg. C and the high pressure of 5.5 GPa. The thermal expansion in the c direction is large and linear with an expansion coefficient of 35.86 x 10 -6 K -1 up to 1000 deg. C, while in the basal plane, the a dimension displays a slight linear contraction up to 750 deg. C with a contraction coefficient of -8.76 x 10 -7 K -1 , but above 750 deg. C a linear expansion is observed with a larger expansion coefficient of 1.52 x 10 -6 K -1

Synthesis and Antimicrobial Activity of Some Novel Substituted Piperazinyl-quinazolin-3(4H-ones

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N. M. Raghavendra

2008-01-01

Full Text Available Several substituted-quinazolin-3(4H-ones were synthesized by condensation of 2-chloro-N-(4-oxo-substituted-quinazolin-3(4H-yl-acetamides with various substituted piperazines through single step reaction. Elemental analysis, IR, 1HNMR and mass spectral data confirmed the structure of the newly synthesized compounds. Synthesized quinazolin-4-one derivatives were investigated for their antibacterial and antifungal activities.

Facile synthesis and herbicidal evaluation of 2-aryl-4h-3, 1-benzoxazin-4-ones

International Nuclear Information System (INIS)

Hussain, Z.; Khan, Z.A.

2013-01-01

The present work deals with the synthesis of 4H-3,1-benzoxazin-4-ones carrying an aryl functional group at position-2. Synthesized compounds tested for herbicidal activity at three different doses (500 micro g/mL, 50 micro g/mL and 5 micro g/mL). Most of the compounds exhibited significant herbicidal activity against Lemna aequinocitalis welv at higher dose (500 micro g/mL). Among the tested compounds 2-phenyl-4H-3,1-benzoxazin-4-one (3a) and 2-(3-chlorophenyl)-4H-3,1-benzoxazin-4-one (3l) completely inhibited the plant growth at 500 and 50 micro g/mL concentrations. All the synthetic compounds were characterized by FT-IR, 1H NMR, EI-MS and elemental analysis. (author)

SYNTHESIZING DERIVATIVES FROM CYCLOPENTANONE ANALOGUE CURCUMIN AND THEIR TOXIC, ANTIOXIDANT AND ANTI-INFLAMMATORY ACTIVITIES

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Adel Zamri1

2011-11-01

Full Text Available Three types of cyclopentanone derivatives have been synthesized from aromatic aldehyde and ketone derivatives undera base condition through aldol condensation. These cyclopentanone products were 2,5-dibenzylidene-cyclopentanone(a, 2,5-bis-(4-hydroxy-benzylidene-cyclopentanone (b, and 2,5-bis-(4-hydroxy-benzylidene-cyclopentanone (cwhich has a yield of 63-99%. The chemical structure of these compounds were determined using UV, IR and NMRspectroscopy. In order to clarify the role of hydroxyl and amine moieties, toxic, antioxidant and anti-inflammatoryactivities were carried out. The toxic test indicated that the compounds showed strong toxicity. In addition, the presenceof hydroxyl and amine groups on both rings of curcumin increased the antioxidant and anti-inflammatory activities

Synthesis, spectral characterization, and pharmacological screening of some 4-[{1-(arylmethylidene}-amino]-3-(4-pyridyl-5-mercapto-4H-1,2,4-triazole derivatives

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Anees A Siddiqui

2010-01-01

Full Text Available Background : Pain is an unpleasant and subjective sensation that results from a harmful sensorial stimulation, which alerts the body about current or potential damage to its tissues and organs. Fever is a complex physiological response triggered by infections or aseptic stimuli. Elevation in body temperature occurs when the concentration of prostaglandin E 2 (PGE 2 increases within parts of the brain. Triazole derivatives have been found to possess various pharmacological and biological activities, such as, anti-inflammatory, analgesics, antipyretic, and antifungal. Materials and Methods : Various 4-[{1-(arylmethylidene}-amino]-3-(4-pyridyl-5-mercapto-4H-1,2,4-triazole derivatives were synthesized by a sequence of reactions starting from isonicotinic acid hydrazide. The synthesized compounds were screened for in-vivo analgesic by the tail-flick method and anti-pyretic activities at a dose of 25 and 100 mg/kg body weight respectively. The antipyretic activity was evaluated using Brewer′s yeast induced pyrexia in rats. Fever was induced by subcutaneously injecting 20 ml/kg of 20% aqueous suspension of Brewer′s yeast in normal saline. Results and Discussion : The analgesic screening results revealed that the compounds 3b, 3c, and 3d exhibited excellent analgesic activity at 60 and 90 minutes compared to the standard drug (Analgin. Results revealed that the compounds 3a, 3e, and 3f significantly decreased the temperature of pyretic (P<0.001 rats at one, three and six hours after compound administration as compared to Aspirin (standard drug. Conclusion : Compounds 3b, 3c, and 3d exhibited significant analgesic activity comparable with the standard drug analgin, using the tail flick model. Compounds 3a, 3e, and 3f showed significant anti-pyretic activities comparable with the standard drug aspirin using the yeast-induced pyrexia model.

synthesis and labelling of some nitrogenous heterocyclic compounds

International Nuclear Information System (INIS)

Mahmoud, A.A.L.

2002-01-01

the imidazole nucleus has wide range of pharmaceutical activities . also , radioiodinated compounds are used in nuclear medicine. this thesis deals with the synthesis of 2-(iodophenyl)-4-oxazoline-5-ons e, which are used as starting materials in the synthesis of the corresponding imidazolinone derivatives. also, it deals with radioiodination f the synthesized compounds to evaluate their application in nuclear medicine. interaction of o- iodo hippuric acid (I) with aromatic aldehydes (i.e., benzaldehyde, p- methoxybenzaldehyde and p- nitrobenzaldehyde) in acetic anhydride and in the presence of fused sodium acetate effected cyclization to afford the corresponding 2-(2-iodophenyl)-4-arylidene- 2-oxazoline-5-ones(l l a-c )

Characterization of rhenium compounds obtained by electrochemical synthesis after aging process

Energy Technology Data Exchange (ETDEWEB)

Vargas-Uscategui, Alejandro, E-mail: avargasuscat@ing.uchile.cl [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); Mosquera, Edgar [Laboratorio de Materiales a Nanoescala, Departamento de Ciencia de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); López-Encarnación, Juan M. [Department of Mathematics-Physics and Department of Chemistry, University of Puerto Rico at Cayey, 205 Ave. Antonio R. Barceló, Cayey, PR 00736, USA. (Puerto Rico); Chornik, Boris [Departamento de Física, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Blanco Encalada Av. 2008, Santiago (Chile); Katiyar, Ram S. [Department of Physics and Institute for Functional Nanomaterials, University of Puerto Rico San Juan, San Juan, PR 00931-3343 (United States); Cifuentes, Luis [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile)

2014-12-15

The proper identification of the molecular nature of the aged rhenium compound obtained by means of electrodeposition from an alkaline aqueous electrolyte was determined. Chemical, structural and vibrational experimental characterization of the aged Re compound showed agreement with quantum-computations, thereby allowing the unambiguous identification of the Re compound as H(ReO{sub 4})H{sub 2}O. - Graphical abstract: Rhenium oxides were electrodeposited on a copper surface and after environmental aging was formed the H(ReO{sub 4})H{sub 2}O compound. The characterization of the synthesized material was made through the comparison of experimental evidence with quantum mechanical computations carried out by means of density functional theory (DFT). - Highlights: • Aged rhenium compound obtained by means of electrodeposition was studied. • The study was made by combining experimental and DFT-computational information. • The aged electrodeposited material is consistent with the H(ReO{sub 4})H{sub 2}O compound.

Synthesis and biological evaluation of biaryl analogs of antitubulin compounds

Energy Technology Data Exchange (ETDEWEB)

Tozatti, Camila Santos Suniga; Khodyuk, Rejane Goncalves Diniz; Silva, Adriano Olimpio da; Santos, Edson dos Anjos dos; Amaral, Marcos Serrou do; Lima, Denis Pires de, E-mail: denis.lima@ufms.br [Centro de Ciencias Exatas e Tecnologia, Universidade Federal de Mato Grosso do Sul, Campo Grande, MS (Brazil); Hamel, Ernest [Screening Technologies Branch, Division of Cancer Treatment and Diagnosis, National Cancer Institute at Frederick, MD (United States)

2012-07-01

This paper reports the synthesis of methanones and esters bearing different substitution patterns as spacer groups between aromatic rings. This series of compounds can be considered phenstatin analogs. Two of the newly synthesized compounds, 5a and 5c, strongly inhibited tubulin polymerization and the binding of [{sup 3}H] colchicine to tubulin, suggesting that, akin to phenstatin and combretastatin A-4, they can bind to tubulin at the colchicine site. (author)

Synthesis and antimicrobial activity of 1-benzhydryl-sulfonyl-4-(3-(piperidin-4-yl) propyl)piperidine derivatives against pathogens of Lycopersicon esculentum: a structure-activity evaluation study.

Science.gov (United States)

Vinaya, K; Kavitha, R; Ananda Kumar, C S; Benaka Prasad, S B; Chandrappa, S; Deepak, S A; Nanjunda Swamy, S; Umesha, S; Rangappa, K S

2009-01-01

Several 1-benzhydryl-sulfonyl-4-(3-(piperidin-4-yl)propyl)piperidine derivatives 8(a-j) were prepared by the treatment of substituted benzhydryl chlorides with 4-(3-(piperidin-4-yl)propyl)piperidine followed by N-sulfonation with sulfonyl chlorides in the presence of dry methylene dichloride and triethyl amine. The synthesized compounds were characterized by (1)H-NMR, IR, and elemental analysis. All the synthesized compounds were evaluated in vitro for their efficacy as antimicrobial agents by artificial inoculation technique against standard strains of two important bacterial viz., Xanthomonas axonopodis pv. vesicatoria and Ralstonia solanacearum as well as and two fungal pathogens namely Alternaria solani and Fusarium solani of tomato plants. We have briefly investigated the structure-activity relation studies and reveal that the nature of substitutions on benzhydryl ring and sulfonamide ring influences the antibacterial activity. Among the synthesized new compounds 8b, 8d, 8g, 8h, 8i, and 8j were showed significant potent antimicrobial activities compared to the standard drugs chloramphenicol, mancozeb.

Rhenium(5) and molybdenum(5) complexes with 4',4(5)-divaleryldibenzo-18-crown-6

International Nuclear Information System (INIS)

Ashurova, N.Kh.; Yakubov, K.G.; Tashmukhamedova, A.K.; Basitova, S.M.

1993-01-01

Methods for synthesizing oxohalide complexes of rhenium and molybdenum with +5 oxidation degree with 4',4 (5) -divaleryldibenzo-18-crown-6 were developed. Content and composition of prepared compounds were investigated by the methods of element analysis, crystal optics, conductometry, IR spectroscopy in the near and far regions, thermogravimetry. Oxidation degree of the complex-forming metal was determined. It was established that composition of the compounds coressponded to the general formula MOLX · H 2 O, where M - Re, Mo; L -4',4 (5) -divaleryldibenzo-18-crown-6; X -Cl - , Br -

[Zn(NH3)4][PtCl6] and [Cd(NH3)4][PtCl6] as precursors for intermetallic compounds PtZn and PtCd

International Nuclear Information System (INIS)

Zadesenets, A.V.; Venediktov, A.B.; Shubin, Yu.V.; Korenev, S.V.

2007-01-01

Double complex salts (tetraamminezinc and tetraamminecadmium hexachloroplatinates) have been synthesized. Their thermal properties have been studied, as well as the products of their degradation in hydrogen and helium atmospheres. Optimal thermolysis schedules have been determined. Thermolysis under hydrogen yields intermetallic compounds PtZn and PtCd [ru

Novel Evaporation Process for Deposition of Kesterite Thin Films Synthesized by Solvothermal Method

Directory of Open Access Journals (Sweden)

J. A. Estrada-Ayub

2017-01-01

Full Text Available Kesterite, a quaternary compound of Cu2ZnSnS4, is a promising option as a material absorber to reduce the cost of photovoltaic solar cells. The solvothermal method is a way to synthesize nanoparticles of this material. In this work, once synthesized, particles were deposited on a substrate through evaporation, and their morphological, structural, and optical properties were studied. Results show that changes of precursor ratios during solvothermal synthesis result in a modification of particle morphology but not on its size. The deposition of already synthesized kesterite through evaporation preserves kesterite structure and permits the formation of a homogenous film on a substrate. Optical reflectance and transmittance measurements allowed estimating the band-gap energy between 1.41 and 1.46 eV for representative samples, which is near the optimum for the absorber material.

Search for new potential anticonvulsants with anxiolytic and antidepressant properties among derivatives of 4,4-diphenylpyrrolidin-2-one.

Science.gov (United States)

Malawska, Katarzyna; Rak, Aleksandra; Gryzło, Beata; Sałat, Kinga; Michałowska, Małgorzata; Żmudzka, Elżbieta; Lodarski, Krzysztof; Malawska, Barbara; Kulig, Katarzyna

2017-02-01

The aim of this study was to synthesize a series of new N-Mannich bases derived from 4,4-diphenylpyrrolidin-2-one having differently substituted 4-phenylpiperazines as potential anticonvulsant agents with additional (beneficial) pharmacological properties. The target compounds 8-12 were prepared in one step from the 4-substituted phenylpiperazines, paraformaldehyde, and synthesized 4,4-diphenylpyrrolodin-2-one (7) by a Mannich-type reaction. The obtained compounds were assessed and tested for their anticonvulsant activity in two screening mouse models of seizures, i.e., the maximal electroshock (MES) test and in the subcutaneous pentylenetetrazole (scPTZ) test. The effect of these compounds on animals' motor coordination was measured in the rotarod test. A selected 4,4-diphenyl-1-((4-phenylpiperazin-1-yl)methyl)pyrrolidin-2-one (8) was evaluated in vivo for its anxiolytic- and antidepressant-like properties. Its impact on animals' locomotor activity was also evaluated. Compound 8 showed protection (25%) in the MES and in the scPTZ tests at the dose of 100mg/kg and was not neurotoxic. In the four-plate test, compound 8 at the dose of 30mg/kg showed a statistically significant (p<0.05) anxiolytic-like activity. In the forced swim test, it reduced the immobility time by 24.3% (significant at p<0.05), which indicates its potential antidepressant-like properties. In the locomotor activity test, compound 8 significantly reduced animals' locomotor activity by 79.9%. The results obtained make a new derivative of 4,4-diphenyl-1-((4-phenylpiperazin-1-yl)methyl)pyrrolidin-2-one (8) a promising lead structure for further development. Copyright © 2016. Published by Elsevier Urban & Partner Sp. z o.o.

Syntheses, Protonation Constants and Antimicrobial Activity of 2 ...

African Journals Online (AJOL)

carboxaldehyde and N-alkylimidazole-2-methanol derivatives [alkyl = benzyl, methyl, ethyl, propyl, butyl, heptyl, octyl and decyl] have been synthesized and the protonation constants determined. The antimicrobial properties of the compounds were tested ...

N-2,4-Dichlorobenzoyl phosphoric triamides: Synthesis ...

Indian Academy of Sciences (India)

Administrator

J (PNCH) for enantiotopic and diastereotopic benzylic. CH2 protons in compounds 7 and 8. The spectroscopic data of newly synthesized compounds were com- pared with those related N-benzoyl derivatives. The structures of compounds 5, 8 and 10 (2,4-Cl2-. C6H3C(O)NHP(O)[NCH2CH(CH3)2]2) have been determined ...

Rhenium(5) and molybdenum(5) complexes with 4',4[sup (]5[sup )]-divaleryldibenzo-18-crown-6. Kompleksnye soedineniya reniya(5) i molibdena(5) s 4',4[sup (]5[sup )]-divalerildibenzo-18-kraun-6

Energy Technology Data Exchange (ETDEWEB)

Ashurova, N Kh; Yakubov, K G; Tashmukhamedova, A K; Basitova, S M [Tadzhikskij Gosudarstvennyj Univ., Dushanbe (Tajikistan)

1993-02-01

Methods for synthesizing oxohalide complexes of rhenium and molybdenum with +5 oxidation degree with 4',4[sup (5)]-divaleryldibenzo-18-crown-6 were developed. Content and composition of prepared compounds were investigated by the methods of element analysis, crystal optics, conductometry, IR spectroscopy in the near and far regions, thermogravimetry. Oxidation degree of the complex-forming metal was determined. It was established that composition of the compounds coressponded to the general formula MOLX [sub [center dot

PP32 and SET/TAF-Iβ proteins regulate the acetylation of newly synthesized histone H4.

Science.gov (United States)

Saavedra, Francisco; Rivera, Carlos; Rivas, Elizabeth; Merino, Paola; Garrido, Daniel; Hernández, Sergio; Forné, Ignasi; Vassias, Isabelle; Gurard-Levin, Zachary A; Alfaro, Iván E; Imhof, Axel; Almouzni, Geneviève; Loyola, Alejandra

2017-11-16

Newly synthesized histones H3 and H4 undergo a cascade of maturation steps to achieve proper folding and to establish post-translational modifications prior to chromatin deposition. Acetylation of H4 on lysines 5 and 12 by the HAT1 acetyltransferase is observed late in the histone maturation cascade. A key question is to understand how to establish and regulate the distinct timing of sequential modifications and their biological significance. Here, we perform proteomic analysis of the newly synthesized histone H4 complex at the earliest time point in the cascade. In addition to known binding partners Hsp90 and Hsp70, we also identify for the first time two subunits of the histone acetyltransferase inhibitor complex (INHAT): PP32 and SET/TAF-Iβ. We show that both proteins function to prevent HAT1-mediated H4 acetylation in vitro. When PP32 and SET/TAF-Iβ protein levels are down-regulated in vivo, we detect hyperacetylation on lysines 5 and 12 and other H4 lysine residues. Notably, aberrantly acetylated H4 is less stable and this reduces the interaction with Hsp90. As a consequence, PP32 and SET/TAF-Iβ depleted cells show an S-phase arrest. Our data demonstrate a novel function of PP32 and SET/TAF-Iβ and provide new insight into the mechanisms regulating acetylation of newly synthesized histone H4. © The Author(s) 2017. Published by Oxford University Press on behalf of Nucleic Acids Research.

Synthesis of Novel Antibacterial Agents: 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-Diones

Directory of Open Access Journals (Sweden)

J. I. Sheikh

2009-01-01

Full Text Available 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-diones(3a-h have been synthesized by a simple and convenient method employing Baker-Venkatraman transformation on 2-aroyloxy-4-hydroxy-5-chloroacetophenones (2a-h with NaOH in dimethylsuphoxide regardless of pyridine. The structures of the synthesized compounds have been assigned on the basis of elemental and spectral analyses (IR, 1HNMR, 13C NMR, Mass. The synthesized compounds were evaluated for the antibacterial efficacy against gram negative and gram positive bacteria.

Bimetallic NiFe2O4 synthesized via confined carburization in NiFe-MOFs for efficient oxygen evolution reaction

Science.gov (United States)

Fang, Zhiqiang; Hao, Zhaomin; Dong, Qingsong; Cui, Yong

2018-04-01

Transition metal oxides that derived from metal-organic framework (MOF) precursor have intensively received attention because of their numerous electrochemical applications. Bimetallic Ni-Fe oxides have been rarely reported on the basis of MOF-related strategy. Herein, a bimetallic NiFe2O4 was successfully synthesized via confined carburization in NiFe-MOF precursors and characterized by XRD, XPS, SEM, and TEM. After conducting an investigation of oxygen evolution reaction (OER), the as-synthesized NiFe2O4 material exhibited good catalytic efficiency and high stability and durability in alkaline media. The as-synthesized NiFe2O4 material would promote the development of MOFs in non-noble-metal OER catalyst.

Divergent Total Syntheses of (-)-Huperzine Q, (+)-Lycopladine B, (+)-Lycopladine C, and (-)-4-epi-Lycopladine D.

Science.gov (United States)

Hong, Benke; Hu, Dachao; Wu, Jinbao; Zhang, Jing; Li, Houhua; Pan, Yingming; Lei, Xiaoguang

2017-07-04

We report herein our synthetic efforts towards the divergent syntheses of (-)-huperzine Q (1), (+)-lycopladine B (2), (+)-lycopladine C (3), and (-)-lycopladine D (4). The 10-step total synthesis of (-)-huperzine Q (1) and the first total syntheses of (+)-lycopladines B (2) and C (3) were accomplished through a series of cascade reactions. Our approach involved a Michael addition/aldol/intramolecular C-alkylation sequence to forge the 6/9 spirocycle ring, and this was followed by an ethylene-accelerated carbonyl-olefin metathesis to construct the common 6/5/9 ring system. Finally, late-stage enamine bromofunctionalization enabled us to access (-)-huperzine Q (1), (+)-lycopladine B (2), and (+)-lycopladine C (3), and a tandem C4-epimerization/retro-Claisen condensation furnished (-)-4-epi-lycopladine D (63). © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metal chloride precursor synthesization of Cu{sub 2}ZnSnS{sub 4} solar cell materials

Energy Technology Data Exchange (ETDEWEB)

Yeh, Min-Yen; Huang, Yu-Fong; Huang, Cheng-Liang; Yang, Chyi-Da [National Kaohsiung Marine University, Kaohsiung, Taiwan (China); Wuu, Dong-Sing [National Chung Hsing University, Taichung, Taiwan (China); Lei, Po-Hsun [National Formosa University, Yunlin, Taiwan (China)

2014-07-15

Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films with kesterite structures were prepared by directly sol-gel synthesizing spin-coated precursors on soda-lime-glass (SLG) substrates. The CZTS precursors were prepared by using solutions of copper (II) chloride, zinc (II) chloride, tin (IV) chloride, and thiourea. The ratio of SnCl{sub 4} in the precursors was found to play a critical role in the synthesization of CZTS. CZTS phases of SnS and SnS{sub 2} were observed in the synthesized films as prepared using precursors with a close to stoichiometric ratio of CuCl{sub 2}:ZnCl{sub 2}:SnCl{sub 4}:CH{sub 4}N{sub 2}S = 4:1:1:8, where SnCl{sub 4} was 1 mol/l. The amounts of the educed SnS and SnS{sub 2} phases observed in the SEM images could be readily reduced by decreasing the volume of SnCl{sub 4} in the mixed solution. With decreasing amount of SnCl{sub 4} from 1 mol/l, the as prepared CZTS reveals a significant improvement in its crystalline properties. In this work, CZTS with an average absorption coefficient and an optical energy gap of over 10{sup 4} cm{sup -1} and ∼1.5 eV, respectively, was obtained using precursors of copper (II) chloride, zinc (II) chloride, tin (IV) chloride, and thiourea mixed in a ratio of 2:1:0.25:8, and it had good crystallinity revealing a Cu-poor composition.

Syntheses, structures and luminescent properties of lanthanide coordination polymers assembled from imidazophenanthroline derivative and oxalate ligands

International Nuclear Information System (INIS)

Zhao, Hui; Sun, Xiao-Xia; Hu, Huai-Ming; An, Ran; Yang, Meng-Lin; Xue, Ganglin

2017-01-01

Nine new lanthanide coordination polymers, namely, [Ln(Hsfpip)(ox) 0.5 (H 2 O)] n ·2n(H 2 O) ((Ln=Eu (1), Tb (2), Dy (3), Ho (4), Er (5), Yb (6), Y(7)), [Ln(H 2 sfpip)(ox)(H 2 O) 4 ] n ·2n(H 2 O) (Ln=Nd (8) Sm (9)), [H 2 ox=oxalic acid, H 3 sfpip=2-(2,4-disulfophenyl)imidazo(4,5-f)(1,10)-phenanthroline] have been synthesized under hydrothermal conditions and characterized by IR spectra, elemental analysis, powder X-ray diffraction and single crystal X-ray diffraction. When sodium oxalate is added, the reactions of lanthanide ions with H 3 sfpip resulted in two types of structures. Compounds 1–7 are obtained at pH 5.0 and exhibit 3D tfz-d networks with ox 2− anions as linkers to bridge the adjacent layers. Compounds 8–9 are obtained at pH 2.0, and display a 1D chain which is further extended to a 3D supramolecular framework through intermolecular hydrogen bonds and π-π interactions. The structural variation from compounds 1–7 to 8–9 can attribute to the pH effect on construction of lanthanide coordination polymers. Moreover, the thermal stabilities and luminescence properties of 1–9 were also investigated. - Graphical abstract: Nine new lanthanide coordination polymers have been synthesized under hydrothermal conditions. Compounds 1–7 exhibit a 3D tfz-d network. Compounds 8–9 display a 1D chain structure. The structural variation from compounds 1–7 to 8–9 can attribute to the pH effect on construction of lanthanide coordination polymers. - Highlights: • Nine lanthanide coordination polymers were prepared under hydrothermal conditions. • Their crystal structures have been determined. • The luminescence and thermal stabilities were studied in the solid state.

Syntheses, structures and luminescent properties of lanthanide coordination polymers assembled from imidazophenanthroline derivative and oxalate ligands

Energy Technology Data Exchange (ETDEWEB)

Zhao, Hui; Sun, Xiao-Xia; Hu, Huai-Ming, E-mail: ChemHu1@NWU.EDU.CN; An, Ran; Yang, Meng-Lin; Xue, Ganglin

2017-01-15

Nine new lanthanide coordination polymers, namely, [Ln(Hsfpip)(ox){sub 0.5}(H{sub 2}O)]{sub n}·2n(H{sub 2}O) ((Ln=Eu (1), Tb (2), Dy (3), Ho (4), Er (5), Yb (6), Y(7)), [Ln(H{sub 2}sfpip)(ox)(H{sub 2}O){sub 4}]{sub n}·2n(H{sub 2}O) (Ln=Nd (8) Sm (9)), [H{sub 2}ox=oxalic acid, H{sub 3}sfpip=2-(2,4-disulfophenyl)imidazo(4,5-f)(1,10)-phenanthroline] have been synthesized under hydrothermal conditions and characterized by IR spectra, elemental analysis, powder X-ray diffraction and single crystal X-ray diffraction. When sodium oxalate is added, the reactions of lanthanide ions with H{sub 3}sfpip resulted in two types of structures. Compounds 1–7 are obtained at pH 5.0 and exhibit 3D tfz-d networks with ox{sup 2−} anions as linkers to bridge the adjacent layers. Compounds 8–9 are obtained at pH 2.0, and display a 1D chain which is further extended to a 3D supramolecular framework through intermolecular hydrogen bonds and π-π interactions. The structural variation from compounds 1–7 to 8–9 can attribute to the pH effect on construction of lanthanide coordination polymers. Moreover, the thermal stabilities and luminescence properties of 1–9 were also investigated. - Graphical abstract: Nine new lanthanide coordination polymers have been synthesized under hydrothermal conditions. Compounds 1–7 exhibit a 3D tfz-d network. Compounds 8–9 display a 1D chain structure. The structural variation from compounds 1–7 to 8–9 can attribute to the pH effect on construction of lanthanide coordination polymers. - Highlights: • Nine lanthanide coordination polymers were prepared under hydrothermal conditions. • Their crystal structures have been determined. • The luminescence and thermal stabilities were studied in the solid state.

Structural, dielectric and conductivity studies of LiNi0.75Mg0.25-xCuxPO4 synthesized by solid state reaction method

Directory of Open Access Journals (Sweden)

Kotamalige Anand

2016-03-01

Full Text Available The olivine structured LiNi0.75Mg0.25-xCuxPO4 (x = 0, 0.05 and 0.1 cathode materials were synthesized by solid state reaction method. The XRD, FTIR and FESEM studies were conducted to investigate the phase purity, crystal structure, lattice parameters and morphology, respectively. The powder X-ray diffraction studies confirmed the single phase formation of the pure and doped compounds which are found to be orthorhombic with the parent LiNiPO4. Morphology and grain sizes of the materials were investigated through FESEM. The FTIR technique was used to characterize the stretching and bending vibrational modes of different functional groups existing in the materials. The cathode properties were analysed through impedance spectroscopy and indicated on improved electrical properties of the doped samples as compared to the pure LiNiPO4. The conductivity and modulus analyses of the samples were carried out at different temperatures and frequencies using the complex impedance spectroscopy technique.

Syntheses, Crystal Structures and Bioactivities of Two Novel Isatin Derivatives

Institute of Scientific and Technical Information of China (English)

SHANG Jian-li; LI Hui-dong; SHANG Jun; SONG Hai-bin; LI Zheng-ming; WANG Jian-guo

2011-01-01

Two novel compoundsl-(4-fluorobenzyl)-4-chloro-(Z)-3-benzoylhydrazono-2-indolinone(1) and 1-(4-methoxybenzyl)-(Z)-3-benzoylhydrazono-2-indolinone(2) were synthesized and their crystal structures were determined by single-crystal X-ray diffraction.Compound 1(C22H15ClFN3O2) crystallized in the triclinic system,space group P1- with a=0.94198(19) nm,b=1.4339(3) nm,c=1.5018(3) nm,a=101.58(3)°,β=102.96(3)°,γ=102.73°,V=1.8602(6) nm3,Mr=407.82,Dc=1.456 g/cm3,μ=0.240 mm-1,F(000)=840,Z=4,R1=0.0442 and wR2=0.1064.Compound 2(C23H19N3O3) crystallized in the triclinic system,space group P1- with a=1.0022(2) nm,b=1.0192(2) nm,c=1.0461(2) nm,a=99.86(3)°,β=117.30(3)°,γ=94.13(3)°,V=0.9215(3) nm3,Mr=385.41,Dc=1.389 g/cm3,μ=0.094mm-1,F(000)=404,Z=2,R1=0.0403 and wR2=0.1142.The preliminary herbicidal activities of the two compounds were also evaluated.

The Exploration and Analysis of the Magnetic Relaxation Behavior in Three Isostructural Cyano-Bridged 3d–4f Linear Heterotrinuclear Compounds

Directory of Open Access Journals (Sweden)

Xia Xiong

2018-03-01

Full Text Available Three isostructural cyano-bridged 3d–4f linear heterotrinuclear compounds, (H2.5O4{Ln[TM(CN5(CNH0.5]2(HMPA4} (Ln = YIII, TM = [FeIII]LS (1; Ln = DyIII, TM = [FeIII]LS (2; Ln = DyIII, TM = CoIII (3, have been synthesized and characterized by single-crystal X-ray diffraction. Due to the steric effect of the HMPA ligands, the central lanthanide ions in these compounds possess a low coordination number, six-coordinate, exhibiting a coordination geometry of an axially elongated octahedron with a perfect D4h symmetry. Four HMPA ligands situate in the equatorial plane around the central lanthanide ions, and two [TM(CN5(CNH0.5]2.5− entities occupy the apical positions to form a cyano-bridged 3d–4f linear heterotrinuclear structure. The static magnetic analysis of the three compounds indicated a paramagnetic behavior of compounds 1 and 3, and possible small magnetic interactions between the intramolecular DyIII and [FeIII]LS ions in compound 2. Under zero dc field, the ac magnetic measurements on 2 and 3 revealed the in-phase component (χ′ of the ac susceptibility without frequency dependence and silent out-of-phase component (χ″, which was attributed to the QTM effect induced by the coordination geometry of an axially elongated octahedron for the DyIII ion. Even under a 1 kOe applied dc field, the χ″ components of 2 were revealed frequency dependence without peaks above 2 K. And under a 2 kOe and 3 kOe dc field, the χ″ components of 3 exhibited weak frequency dependence below 4 K with the absence of well-shaped peaks, which confirmed the poor single-ion magnetic relaxation behavior of the six-coordinate DyIII ion excluding any influence from the neighboring [FeIII]LS ions as that in the analogue 2.

Synthesis, antifungal evaluation and in silico study of novel Schiff bases derived from 4-amino-5(3,5-dimethoxy-phenyl-4H-1,2,4-triazol-3-thiol

Directory of Open Access Journals (Sweden)

N.S. Hari Narayana Moorthy

2017-05-01

Full Text Available A novel series of Schiff bases based on of 4-amino-5-(3,5-dimethoxy-phenyl-4H-1,2,4-triazol-3-thiol scaffold was prepared by heating thiocarbohydrazide and 3,5,-dimethoxy benzoic acid at the temperature above its meting point, and subsequently, treating with substituted benzaldehydes. The chemical constituents in the synthesized compounds were confirmed by IR, Mass, 1H NMR spectroscopy and elemental analysis and the antifungal activity was evaluated against Candida albicans. The structure activity relationship analysis shows that the chloride substituted derivatives possess promising activity in micromolar concentration and also the hydroxy phenyl derivatives exhibited considerable activity at 128 μg/ml. But other compounds with amino, furan and methoxy substitutions did not show antifungal activity till the concentration of 512 μg/ml. In silico pharmacokinetic prediction shows that all the compounds obeyed Lipinski rule of 5 and are free of toxicity and metabolically stable. Pharmacophore analysis revealed that the aromatic/hydrophobic and aromatic/acceptor/donor features in the compounds are essential for the activity. The predicted cardiotoxicity (hERG and lethal effect of the synthesized compounds will permit us to carry out further in vitro and in vivo toxicity studies.

Design and syntheses of hybrid metal-organic materials based on K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] metallotectons

Science.gov (United States)

Sun, Yayong; Zong, Yingxia; Ma, Haoran; Zhang, Ao; Liu, Kang; Wang, Debao; Wang, Wenqiang; Wang, Lei

2016-05-01

By using K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] (C2O42-=oxalate) metallotectons as the starting material, we have synthesized eight novel complexes with formulas [{Fe(C2O4)2(H2O)2}2]·(H-L1)2·H2O 1, [Fe(C2O4)Cl2]·(H2-L2)0.5·(L2)0.5·H2O 2, [{Fe(C2O4)1.5Cl2}2]·(H-L3)43, [Fe2(C2O4)Cl8]·(H2-L4)2·2H2O 4, K[Al(C2O4)3]·(H2-L5)·2H2O 5, K[Al(C2O4)3]·(H-L6)2·2H2O 6, K[Cr(C2O4)3]·2H2O 7, Na[Fe(C2O4)3]·(H-L6)2·2H2O 8 (with L1=4-dimethylaminopyridine, L2=2,3,5,6-tetramethylpyrazine, L3=2-aminobenzimidazole, L4=1,4-bis-(1H-imidazol-1-yl)benzene, L5=1,4-bis((2-methylimidazol-1-yl)methyl)benzene, L6=2-methylbenzimidazole). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra and thermogravimetric analyses. Compound 3 is a 2D H-bonded supramolecular architecture. Others are 3D supramolecular structures. Compound 1 shows a [Fe(C2O4)2(H2O)2]- unit and 3D antionic H-bonded framework. Compound 2 features a [Fe(C2O4)Cl2]- anion and 1D iron-oxalate-iron chain. Compound 3 features a [Fe2(C2O4)3Cl4]4- unit. Compound 4 features distinct [Fe2(C2O4)Cl8]4- units, which are mutual linked by water molecules to generated a 2D H-bonded network. Compound 5 features infinite ladder-like chains constructed by [Al(C2O4)3]3- units and K+ cations. The 1D chains are further extended into 3D antionic H-bonded framework through O-H···O H-bonds. Compounds 6-8 show 2D [KAl(C2O4)3]2- layer, [KCr(C2O4)3]2- layer and [NaFe(C2O4)3]2- layer, respectively.

4-GHz counters bring synthesizers up to speed

Science.gov (United States)

Lee, F.; Miller, R.

1984-06-01

The availability of digital IC counters built on GaAs makes direct frequency division in microwave synthesizers possible. Four GHz is the highest clock rate achievable in production designs. These devices have the ability to drive TTL/CMOS logic, and the counter can be connected directly to single-chip frequency synthesizers controllers. A complete microwave sythesizer is formed by two chips and a voltage-controlled oscillator (VCO). The advantages of GaAs are discussed along with flip-flop basics, aspects of device fabrication, and the characteristics of GaAs MESAFETs. Attention is given to a GaAs prescaler usable for direct conversion, four kinds of flip-flops in a divide-by-two mode, and seven-stage binary ripple counters.

Hydrazine-hydrothermal method to synthesize three-dimensional chalcogenide framework for photocatalytic hydrogen generation

International Nuclear Information System (INIS)

Liu Yi; Kanhere, Pushkar D.; Wong, Chui Ling; Tian Yuefeng; Feng Yuhua; Boey, Freddy; Wu, Tom; Chen Hongyu; White, Tim J.; Chen Zhong; Zhang Qichun

2010-01-01

A novel chalcogenide, [Mn 2 Sb 2 S 5 (N 2 H 4 ) 3 ] (1), has been synthesized by the hydrazine-hydrothermal method. X-ray crystallography study reveals that the new compound 1 crystallizes in space group P1-bar (no. 2) of the triclinic system. The structure features an open neutral three-dimensional framework, where two-dimensional mesh-like inorganic layers are bridged by intra- and inter-layer hydrazine ligands. Both two Mn1 and Mn2 sites adopt distorted octahedral coordination. While two Sb1 and Sb2 sites exhibit two different coordination geometries, the Sb1 site is coordinated with three S atoms to generate a SbS 3 trigonal-pyramidal geometry, and the Sb2 site adopts a SbS 4 trigonal bipyramidal coordination geometry. It has an optical band gap of about ∼2.09 eV, which was deduced from the diffuse reflectance spectrum, and displays photocatalytic behaviors under visible light irradiation. Magnetic susceptibility measurements show compound 1 obeys the Curie-Weiss law in the range of 50-300 K. -- Graphical abstract: A novel chalcogenide, [Mn 2 Sb 2 S 5 (N 2 H 4 ) 3 ] (1), synthesized by hydrazine-hydrothermal method, has a band gap of about ∼2.09 eV and displays photocatalytic behaviors under visible light irradiation. Display Omitted

Investigation of the Mesostructure of Transition-Metal Monogermanides Synthesized under Pressure

Science.gov (United States)

Safiulina, I. A.; Altynbaev, E. V.; Iashina, E. G.; Heinemann, A.; Fomicheva, L. N.; Tsvyashchenko, A. V.; Grigoriev, S. V.

2018-04-01

The mesostructure of transition-metal monogermanides Mn1 - x Co x Ge is studied by small-angle neutron scattering in a wide range of concentrations x = 0-0.95. These compounds were synthesized under high pressure and are metastable under normal conditions. The experimental dependences I( Q) obtained for the whole series of samples in the range of transferred momenta (6 × 10-2 nm-1 interesting to note that such defects are absent in the isostructural FeGe compound, i.e., the experimental dependences of the intensity are described well by the expression Q - n with an exponent n = 4.1 ± 0.1, which demonstrates the presence of crystallites with a uniform density distribution inside and a sharp boundary characterizing the surface.

Recent Syntheses of 1,2,3,4-Tetrahydroquinolines, 2,3-Dihydro-4(1H-quinolinones and 4(1H-Quinolinones using Domino Reactions

Directory of Open Access Journals (Sweden)

Baskar Nammalwar

2013-12-01

Full Text Available A review of the recent literature is given focusing on synthetic approaches to 1,2,3,4-tetrahydroquinolines, 2,3-dihydro-4(1H-quinolinones and 4(1H-quinolinones using domino reactions. These syntheses involve: (1 reduction or oxidation followed by cyclization; (2 SNAr-terminated sequences; (3 acid-catalyzed ring closures or rearrangements; (4 high temperature cyclizations and (5 metal-promoted processes as well as several less thoroughly studied reactions. Each domino method is presented with a brief discussion of mechanism, scope, yields, simplicity and potential utility.

Synthesis of 6-Methyl-9-propyldibenzothiophene-4-ol amended to 9-isopropyl-6-methyldibenzothiophene-4-ol. Final technical report, July 25, 1991--January 25, 1993

Energy Technology Data Exchange (ETDEWEB)

Eisenbraun, E.J.

1992-02-17

This is a draft final technical report on Task 1 of a contract to synthesize 6-Methyl-9-propyldibenzothiophene-4-ol, as amended to 9- isopropyl-6-methyldibenzothiophene-4-ol. This report is a compilation of data presented in earlier reports. The first annual report dealt with an attempted synthesis of 4-methoxy-6-methyl-9- propyldibenzothiophene (the original target compound), the successful synthesis and delivery of 200 grams of the sulfide 1,4-diethyl-2- [(2{prime}-methoxyphenyl)-thio]benzene, and initial work on a new synthesis route for the preparation of the new target compound 9- isopropyl-6-methyldibenzothiophene-4-ol. The change to the new target compound and the new synthesis route became necessary when it was learned that the sulfide mixture could not be cyclized to the substituted dibenzothiophene mixture. The second annual report described the successful preparation of 45 g of the new target compound using the new synthesis route. Subsequently funds were provided to synthesize an additional 45 g of the new target using the same reaction scheme. This task was recently completed.

Synthesis of 4-Triazolylamino- and 4-Benzothiazolylamino-3-nitro-2H-[1]-Benzopyran-2-ones and their Antimicrobial Activity

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Ramiz Hoti

2014-10-01

Full Text Available Novel substituted benzopyran-2-one derivatives were synthesized by catalytic condensation reactions under reflux conditions. 4-(1,2,4-Triazolyl-3-amino-3-nitro-2H-[1]-benzopyran-2-ones 4(a-b were synthesized by condensation of 4-chloro-3-nitro-2H-[1]-benzopyran-2-one (2 and corresponding 3-aminotriazoles 3(a-b. 4-(4’-methoxy-2-benzothiazolylamino-3-nitro-2H-[1]-benzopyran-2-one (4c, 4-(6’-nitro-2-benzothiazolylamino-3-nitro-2H-[1]-benzopyiran-2-one (4d and 4-(6’-fluoro-2-benzothiazolylamino-3-nitro-2H-[1]-benzopyran-2-one (4e were synthesized by condensation of 4-chloro-3-nitro-2H-[1]-benzopyran-2-one (2 and corresponding 2-aminobenzothiazole 3(c-e under reflux reaction conditions. Further, alkali hydrolysis of 4(a-e afforded the 2-hydroxy-ω-nitroacetophenone (5. Antimicrobial activity of products 4(a-e against S. aurous, E. coli and Klebsiella were investigated measuring of inhibition zones around the discs which are marked with DMF, concentration 2 mg/mL, 4 mg/mL and 6 mg/mL solutions. Compounds 4c, 4e and 4d were more active against S. aureus. Emphatic activity against E. coli exhibited compounds 4b and 4e, whereas 4c and 4d were more active against Klebsiella.

Synthesis, crystal structure and biological activity of n-(5-(o-tolyl)-1, 3, 4-thiadiazol-2-yl)cyclopropanecarboxamide

International Nuclear Information System (INIS)

Tong, J.Y.; Sun, N.B.; Wu, H.K.

2013-01-01

A new 1, 3, 4-thiadiazole compound, N-(5-(o-tolyl)-1,3,4-thiadiazol-2-yl) cyclopropanecarboxamide, was synthesized and its structure was confirmed by 1H NMR, MS and HRMS. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has moderate herbicidal activity against Brassica campestris and fungicidal activities against Sclerotinia sclerotiorum(Lib.) de Bary, Rhizoctonia solanii, Fusarium oxysporum, Corynespora cassiicola, and Botrytis cinerea. (author)

Syntheses of cytotoxic novel arctigenin derivatives bearing halogen and alkyl groups on aromatic rings.

Science.gov (United States)

Yamauchi, Satoshi; Wukirsari, Tuti; Ochi, Yoshiaki; Nishiwaki, Hisashi; Nishi, Kosuke; Sugahara, Takuya; Akiyama, Koichi; Kishida, Taro

2017-09-01

The new lignano-9,9'-lactones (α,β-dibenzyl-γ-butyrolactone lignans), which showed the higher cytotoxicity than arctigenin, were synthesized. The well-known cytotoxic arctigenin showed activity against HL-60 cells (EC 50 =12μM), however, it was inactive against HeLa cells (EC 50 >100μM). The synthesized (3,4-dichloro, 2'-butoxy)-derivative 55 and (3,4-dichloro, 4'-butyl)-derivative 66 bearing the lignano-9,9'-lactone structures showed the EC 50 values of 10μM and 9.4μM against HL-60 cells, respectively. Against HeLa cells, the EC 50 value of the derivative 66 was 27μM. By comparing the activities with the corresponding 9,9'-epoxy structure (tetrahydrofuran compounds), the importance of the lactone structure of 55 and 66 for the higher activities was shown. The substituents on the aromatic ring of the lignano-9,9'-lactones affected the cytotoxicity level, observing more than 10-fold difference. Copyright © 2017. Published by Elsevier Ltd.

Structural investigation of a new antimicrobial thiazolidine compound

Energy Technology Data Exchange (ETDEWEB)

Cozar, I. B.; Pîrnău, A. [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath Street, RO-400293 Cluj-Napoca (Romania); Vedeanu, N.; Nastasă, C. [Iuliu Hatieganu University of Medicine and Pharmacy, Faculty of Pharmacy, RO-400023 Cluj-Napoca (Romania)

2013-11-13

Thiazoles and their derivatives have attracted the interest over the last decades because of their varied biological activities: antibacterial, antiviral, antifungal, inflammation or in the treatment of allergies. A new synthesized compound 3-[2-(4-Methyl-2-phenyl-thiazol-5-yl)-2-oxo-ethyl]-thazolidine-2,4-dione was investigated by FT-IR, FT-Raman, {sup 1}H, {sup 13}C NMR spectroscopies and also by DFT calculations at B3LYP/6-31G(d) level of theory. The very good correlation found between the experimental and theoretical data shows that the optimized molecular structure is very close to reality. Also the NMR spectra show a monomeric behaviour of this compound in solutions.

Synthesis of new derivatives of 1-(3-aminophenyl-4-benzoyl-5-phenyl-1H-pyrazole-3-carboxylic acid

Directory of Open Access Journals (Sweden)

RAHMI KASIMOGULLAR

2010-12-01

Full Text Available 1-(3-Aminophenyl-4-benzoyl-5-phenyl-1H-pyrazole-3-carboxylic acid (1 was synthesized according to the literature. 2-(3-Aminophenyl-2,6-dihydro-3,4-diphenyl-7H-pyrazolo[3,4-d]pyridazin-7-one (5 was obtained by the cyclocondensation reaction of 1 with hydrazine hydrate. New pyrazole derivatives of compounds 1 and 5 were synthesized by their reaction with β-diketones, β-ketoesters, β-naphthol, phenol and various other reagents. The structures of the synthesized compounds were characterized by 1H-NMR, 13C-NMR, IR and mass spectroscopy, as well as elemental analysis.

Synthesis, physical and chemical properties, antihypoxic activity of some 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-N-R1-1,3,4-thiadiazole-2-amines and 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-4-R1-4H-1,2,4-t

Directory of Open Access Journals (Sweden)

V. M. Odyntsova

2018-03-01

Full Text Available Today, an increase of natural and technogenic situations leads to the disorders of the central nervous system, functional-metabolic processes, vascular diseases, in particular, acute cerebral blood flow disorders. In addition, the changes occurring on the molecular and cellular levels are in the basis of the functional violations of individual systems and the organism as a whole. Hypoxia not only complicates the disease course, but in most cases, determines its outcome. The important role in the fight against hypoxia belongs to antioxidants, which improve the circulating oxygen utilization by the body, reduce its need for the organs and tissues, which is not only expedient but necessary for the treatment of many acute and chronic pathological processes. So, the frequency of the hypoxic states and a wide range of factors causing them determine the relevance of new ways and methods finding to overcome the oxygen deficiency. The aim of this work is the purposeful search of some 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-N-R1-1,3,4-thiadiazole-2-amines and 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-4-R1-4H-1,2,4-triazole-3-thiols, the study of their physical and chemical properties and pharmacological screening of the antihypoxic activity of the obtained compounds. Materials and methods. The study of physical and chemical properties was conducted on certified and licensed modern equipment. Antihypoxic activity was studied during the modeling process of hypoxia with hypercapnia. Mexidol was used as a comparison drug in studies at a dose of 100 mg/kg. Results. As the result of the study, it was found that the synthesized compounds and the comparison drug influenced on rats’ life span differently. Compounds, the antihypoxic activity of which exceeded control have been discovered, and others’ were at the level of Mexidol. A number of compounds showed a somewhat less activity in comparison with control, and two

Syntheses, structures and properties of four 3D microporous lanthanide coordination polymers based on 3,5-pyrazoledicarboxylate and oxalate ligands

International Nuclear Information System (INIS)

Song, Juan; Wang, Ji-Jiang; Hu, Huai-Ming; Wu, Qing-Ran; Xie, Juan; Dong, Fa-Xin; Yang, Meng-Lin; Xue, Gang-Lin

2014-01-01

Four three-dimensional lanthanide coordination polymers with reversible structural interconversions, [Ln 2 (Hpdc) 2 (C 2 O 4 )(H 2 O) 4 ] n ·2nH 2 O [Ln=Sm (1), Eu (2), Tb (3) and Dy (4)], have been synthesized by hydrothermal reactions of lanthanide nitrates with 3,5-pyrazoledicarboxylic (H 3 pdc) and oxalic acids. It is noteworthy that there is an in situ reaction in 1, in which H 3 pdc was decomposed into (ox) 2− with Cu(II)–Sm(III) synergistic effect under hydrothermal conditions. These compounds are isostructural and crystallized in the monoclinic P2 1 /c space group. The Ln(III) ions are eight-coordinated with dodecahedron coordination geometry. These polyhedra are linked by oxalate groups to form 1D zigzag chain, which are further connected by 3,5-pyrazoledicarboxylate to extend similar 3D frameworks with channels along c-axis in 1–4. These coordination polymers display the characteristic emission bands of the Ln(III) ions in the solid state and possess good thermal stabilities. - Graphical abstract: Four 3D microporous lanthanide coordination polymers with reversible structural interconversion have been synthesized. They exhibit characteristic emission bands of the lanthanide ions and possess great thermal stability. - Highlights: • Four lanthanide coordination polymers have been hydrothermal synthesized. • There is an in situ reaction in 1 in which H 3 pdc was decomposed into (ox) 2− with the Cu(II)–Sm(III) synergistic effect under hydrothermal conditions. • TGA and XRD studies reveal that upon hydration–dehydration, compounds 1–4 undergo a reversible structural interconversion process through a cooling-heating cycle. • Compounds 1–4 exhibit characteristic lanthanide-centered luminescence

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

Energy Technology Data Exchange (ETDEWEB)

Qian, Cheng [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Kong, Fang [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Mao, Jiang-Gao, E-mail: mjg@fjirsm.ac.cn [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China)

2016-06-15

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy){sub 2}V{sub 2}O{sub 4}(SeO{sub 3}){sub 2} (1), Cu(2,2-bipy)V{sub 2}O{sub 4}(SeO{sub 3}){sub 2}·0.5H{sub 2}O (2) and Cu{sub 2}(2,2-bipy){sub 2}V{sub 5}O{sub 12}(SeO{sub 3}){sub 2} (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy)_2V_2O_4(SeO_3)_2}{sub 2} dimeric cluster composed of two {Ni(2,2-bipy)_2}{sup 2+} moieties connected by the {V_4O_8(SeO_3)_4}{sup 4-} cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V_2O_4(SeO_3)_2}{sub n} chain in which the {Cu_2(2,2-bipy)_2}{sup 4+} moieties are bridged by the {V_4O_8(SeO_3)_4}{sup 4−} clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {V"I"VV"V_4Se"I"V_2O_1_8}{sub n}{sup 4−} and {Cu(2,2-bipy)}{sup 2+} complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V_4O_8(SeO_3)_4}{sup 4−} cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties. - Graphical abstract: We got three new vanadium selenites with organically linked copper/nickel complex, namely, Ni(2,2-bipy){sub 2}V{sub 2}O{sub 4}(SeO{sub 3}){sub 2} (1), Cu(2,2-bipy)V{sub 2}O{sub 4}(SeO{sub 3}){sub 2}·0.5H{sub 2}O (2) and Cu{sub 2}(2,2-bipy){sub 2}V{sub 5}O{sub 12}(SeO{sub 3}){sub 2} (3) by hydrothermally syntheses. They display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. Display Omitted - Highlights: • Three new compounds display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. • The Tetranuclear {V_4O_8(SeO_3)_4}{sup 4−} cluster and the vanadate {V

Thermal stability and microstructure characterization of MgAl{sub 2}O{sub 4} nanoparticles synthesized by reverse microemulsion method

Energy Technology Data Exchange (ETDEWEB)

Fu, Ping; Lu, Wenzhong; Lei, Wen, E-mail: lwz@mail.hust.edu.cn [Department of Electronic Science and Technology, HuaZhong University of Science and Technology - HUST, Wuhan (China); Wu, Ke; Xu, Yong [Department of Materials Science and Engineering, Wuhan Institute of Technology - WIT, Wuhan (China); Wu, Jiamin [Key Lab of Functional Materials for Electronic Information(B) MOE, HuaZhong University of Science and Technology - HUST, Wuhan (China)

2013-11-01

Magnesium aluminate (MgAl{sub 2}O{sub 4}) spinel nanoparticles were synthesized by reverse microemulsion process in cyclohexane by using two kinds of surfactants, n-amyl alcohol as cosurfactant and mixture of aluminic/magnesic salt aqueous solution as basic reagents. The effects of surfactant types and titration methods on the morphologies and sizes of the MgAl{sub 2}O{sub 4} nanoparticles were characterized by TEM, TGA-DTA, XRD, HR-TEM and FT-IR. TEM images show that the particles prepared by forward titration method with SPAN-80/Triton X-100 compound emulsifier have uniform spherical shape and good monodispersity with an average size of 9.5 nm. However, the average size of the particles prepared by reverse-titration method was about 10 nm and some particles have irregular plate like appearance. The products prepared with NP-40 surfactant and forward-titration method were agglomerated with an average size of 13 nm. TGA and XRD results show that the reverse microemulsion method has dramatically lowered the calcination temperature of MgAl{sub 2}O{sub 4} with a degree of 700 Degree-Sign C, and the precursor can transform to single spinel phase at 900 Degree-Sign C. (author)

Electrochemical Study on Newly Synthesized Chlorocurcumin as an Inhibitor for Mild Steel Corrosion in Hydrochloric Acid

Directory of Open Access Journals (Sweden)

Ahmed A. Al-Amiery

2013-11-01

Full Text Available A new curcumin derivative, i.e., (1E,4Z,6E-5-chloro-1,7-bis(4-hydroxy-3-methoxyphenylhepta-1,4,6-trien-3-one (chlorocurcumin, was prepared starting with the natural compound curcumin. The newly synthesized compound was characterized by elemental analysis and spectral studies (IR, 1H-NMR and 13C-NMR. The corrosion inhibition of mild steel in 1 M HCl by chlorocurcumin has been studied using potentiodynamic polarization (PDP measurements and electrochemical impedance spectroscopy (EIS. The inhibition efficiency increases with the concentration of the inhibitor but decreases with increases in temperature. The potentiodynamic polarization reveals that chlorocurcumin is a mixed-type inhibitor. The kinetic parameters for mild steel corrosion were determined and discussed.

Electrochemical Study on Newly Synthesized Chlorocurcumin as an Inhibitor for Mild Steel Corrosion in Hydrochloric Acid

Science.gov (United States)

Al-Amiery, Ahmed A.; Kadhum, Abdul Amir H.; Mohamad, Abu Bakar; Musa, Ahmed Y.; Li, Cheong Jiun

2013-01-01

A new curcumin derivative, i.e., (1E,4Z,6E)-5-chloro-1,7-bis(4-hydroxy-3-methoxyphenyl)hepta-1,4,6-trien-3-one (chlorocurcumin), was prepared starting with the natural compound curcumin. The newly synthesized compound was characterized by elemental analysis and spectral studies (IR, 1H-NMR and 13C-NMR). The corrosion inhibition of mild steel in 1 M HCl by chlorocurcumin has been studied using potentiodynamic polarization (PDP) measurements and electrochemical impedance spectroscopy (EIS). The inhibition efficiency increases with the concentration of the inhibitor but decreases with increases in temperature. The potentiodynamic polarization reveals that chlorocurcumin is a mixed-type inhibitor. The kinetic parameters for mild steel corrosion were determined and discussed. PMID:28788402

Synthesis and antitumoral activity of novel 3-(2-substituted-1,3,4-oxadiazol-5-yl) and 3-(5-substituted-1,2,4-triazol-3-yl) beta-carboline derivatives.

Science.gov (United States)

Formagio, Anelise S Nazari; Tonin, Lilian T Düsman; Foglio, Mary Ann; Madjarof, Christiana; de Carvalho, João Ernesto; da Costa, Willian Ferreira; Cardoso, Flávia P; Sarragiotto, Maria Helena

2008-11-15

Several novel 1-substituted-phenyl beta-carbolines bearing the 2-substituted-1,3,4-oxadiazol-5-yl and 5-substituted-1,2,4-triazol-3-yl groups at C-3 were synthesized and evaluated for their in vitro anticancer activity. The assay results pointed thirteen compounds with growth inhibition effect (GI(50)<100 microM) for all eight different types of human cancer cell lines tested. The beta-carbolines 7a and 7h, bearing the 3-(2-metylthio-1,3,4-oxadiazol-5-yl) group, displayed high selectivity and potent anticancer activity against ovarian cell line with GI(50) values lying in the nanomolar concentration range (GI(50)=10 nM for both compounds). The 1-(N,N-dimethylaminophenyl)-3-(5-thioxo-1,2,4-triazol-3-yl) beta-carboline (8g) was the most active compound, showing particular effectiveness on lung (GI(50)=0.06 microM), ovarian and renal cell lines. The potent anticancer activity presented for synthesized compounds 7a, 7h, and 8g, together with their easiness of synthesis, makes these compounds promising anticancer agents.

Study of bismuth oxide compounds as cathodic materials in lithium accumulators

International Nuclear Information System (INIS)

Apostolova, R.D.; Shembel', E.M.

1999-01-01

Two groups of bismuth oxide base compounds: rare earth bismuthides - SmBiO 3 and EuBiO 3 , as well as the Aurivillius phase - Bi 4 V 2 O 11 , were synthesized and electrochemically studied as novel cathodic materials for high-energy lithium current sources [ru

Synthesis of (E)-N'-[1-(2,4-Dihydroxyphenyl)ethylidene]substituted hydrazides as possible alpha-glucosidase and butyrylcholinesterase Inhibitors

International Nuclear Information System (INIS)

Abbasi, M.A.; Shah, S.A.H.; Siddiqui, S.Z.; Khan, K.M.

2017-01-01

In the current research work, (E)-N'-[1-(2,4-dihydroxyphenyl)ethylidene]substituted hydrazides were synthesized in a couple of steps and their enzyme inhibition potential was analyzed. Firstly 2,4-hydroxyacetophenone (1) was reacted with hydrated hydrazine (2) under stirring to yield (E)-4-(1-hydrazonoethyl)benzene-1,3-diol (3) which was further reacted with different acid halides, (4a-i) to afford (E)-[1-(2,4-dihydroxyphenyl)ethylidene]substituted hydrazides (5a-i). These synthesized compounds were characterized by EI-MS, 1H-NMR spectral techniques and were also evaluated against a-glucosidase and butyrylcholinesterase enzymes. The synthesized compounds were found to be acceptable inhibitors of a-glucosidase and decent inhibition against butyrylcholinesterase. (author)

Crystal structure of 4,4′-bis[3-(piperidin-1-ylprop-1-yn-1-yl]-1,1′-biphenyl

Directory of Open Access Journals (Sweden)

Anqi Walbaum

2017-06-01

Full Text Available The title compound, C28H32N2, (I, is one of a second generation of compounds designed and synthesized based on a very potent and selective α9α10 nicotinic acetylcholine receptor antagonist ZZ161C {1,1′-[[1,1′-biphenyl]-4,4′-diylbis(prop-2-yne-3,1-diyl]bis(3,4-dimethylpyridin-1-ium bromide}, which has shown analgesic effects in a chemotherapy-induced neuropathy animal model. Compound (I was synthesized by the reaction of 4,4′-bis(3-bromoprop-1-yn-1-yl-1,1′-biphenyl with piperidine at room temperature in acetonitrile. The single-crystal used for X-ray analysis was obtained by dissolving (I in a mixture of dichloromethane and methanol, followed by slow evaporation of the solvent. In the crystal of (I, the biphenyl moiety has a twisted conformation, with a dihedral angle of 25.93 (4° between the benzene rings. Both piperidine head groups in (I are in the chair conformation and are oriented so that the N-atom lone pairs of each piperidine group point away from the central biphenyl moiety.

Syntheses, spectroscopic and magnetic properties of polystyrene-anchored coordination compounds of thiazolidinone

Directory of Open Access Journals (Sweden)

D. Kumar

2014-01-01

Full Text Available The reaction between polystyrene 3-formylsalicylate and furoic acid hydrazide in DMF in the presence of ethyl acetate results in the formation of polystyrene N-(2-carbamoylfuranyl-3'-carboxy-2'-hydroxybenzylideneimine (I. A benzene suspension of I reacts with mercaptoacetic acid and forms the polystyrene N-(2-carbamoylfuranyl-C-(3'-carboxy-2'-hydroxyphenylthiazolidin-4-one, PSCH2–LH2 (II. A DMF suspension of II reacts with Mn(II, Ni(II, Cd(II, Fe(III and UO2(VI ions and forms the polystyrene-anchored coordination compounds of the types, [PSCH2–LMn(DMF3], [PSCH2–LNi(DMF3], [PSCH2–LCd(DMF], [PSCH2–LH2FeCl3] and [PSCH2–LHUO2(NO3(DMF]. The polystyrene-anchored coordination compounds have been characterized on the basis of elemental analyses, spectral (IR, reflectance studies and magnetic susceptibility measurements. II acts as a neutral tridentate ONO donor ligand in [PSCH2–LH2FeCl3], a monobasic tridentate ONO donor ligand in [PSCH2–LHUO2(NO3(DMF], a dibasic tridentate ONO donor ligand in [PSCH2–LMn(DMF3], [PSCH2–LNi(DMF3] and [PSCH2–LCd(DMF]. A tetrahedral structure for Cd(II and an octahedral structure for Mn(II, Ni(II, Fe(III and a square-antiprism geometry for UO2(VI complex are suggested. DOI: http://dx.doi.org/10.4314/bcse.v28i1.4

Composite multi-parameter ranking of real and virtual compounds for design of MC4R agonists: renaissance of the Free-Wilson methodology.

Science.gov (United States)

Nilsson, Ingemar; Polla, Magnus O

2012-10-01

Drug design is a multi-parameter task present in the analysis of experimental data for synthesized compounds and in the prediction of new compounds with desired properties. This article describes the implementation of a binned scoring and composite ranking scheme for 11 experimental parameters that were identified as key drivers in the MC4R project. The composite ranking scheme was implemented in an AstraZeneca tool for analysis of project data, thereby providing an immediate re-ranking as new experimental data was added. The automated ranking also highlighted compounds overlooked by the project team. The successful implementation of a composite ranking on experimental data led to the development of an equivalent virtual score, which was based on Free-Wilson models of the parameters from the experimental ranking. The individual Free-Wilson models showed good to high predictive power with a correlation coefficient between 0.45 and 0.97 based on the external test set. The virtual ranking adds value to the selection of compounds for synthesis but error propagation must be controlled. The experimental ranking approach adds significant value, is parameter independent and can be tuned and applied to any drug discovery project.

Simple Syntheses of Two New Benzo-Fused Macrocycles Incorporating Chalcone Moiety.

Science.gov (United States)

Mondal, Rina; Samanta, Swati; Sarkar, Saheli; Mallik, Asok K

2014-01-01

Simple syntheses of the benzo-fused 26-membered macrocyclic bischalcone (19E,43E)-2.11.27.36-tetroxaheptacyclo[44.4.0.0(4,9).0(12,17).0(21,26).0(29,34).0(37,42)]pentaconta-1(46),4(9),5,7,12(17),13,15,19,21,23,25,29,31,33,37,39,41,43,47,49-icosaene-18,45-dione (3) and the benzo-fused 13-membered macrocyclic chalcone (19E)-2.11-dioxatetracyclo[19.4.0.0(4,9).0(12,17)]pentacosa-1(25),4(9),5,7,12(17),13,15,19,21,23-decaen-18-one (5) using very common starting materials and reagents are described. The compounds are new and they have been characterized from their analytical and spectral data.

Syntheses, spectroscopic characterization, crystal structure and natural rubber vulcanization activity of new disulfides derived from sulfonyldithiocarbimates

Science.gov (United States)

Alves, Leandro de Carvalho; Rubinger, Mayura Marques Magalhães; Tavares, Eder do Couto; Janczak, Jan; Pacheco, Elen Beatriz Acordi Vasques; Visconte, Leila Lea Yuan; Oliveira, Marcelo Ribeiro Leite

2013-09-01

The compounds (Bu4N)2[(4-RC6H4SO2NCS2)2] [Bu4N = tetrabutylammonium cation; R = H (1), F (2), Cl (3) and Br (4)] and (Ph4P)2[(4-RC6H4SO2NCS2)2]ṡH2O [Ph4P = tetraphenylphosphonium cation and R = I (5)] were synthesized by the reaction of the potassium dithiocarbimates (4-RC6H4SO2NCS2K2ṡ2H2O) with I2 and Bu4NBr or Ph4PCl. The IR data were consistent with the formation of the dithiocarbimatodisulfides anions. The NMR spectra showed the expected signals for the cations and anions in a 2:1 proportion. The structures of compounds 1-5 were determined by the single crystal X-ray diffraction. The compounds 2, 3 and 4 are isostructural and crystallise in the centrosymmetric space group C2/c of the monoclinic system. Compound 1 crystallises in the monoclinic system in the space group of P21/n and the compound 5 crystallises in the centrosymmetric space group P-1 of the triclinic system. The complex anions of compounds 2, 3 and 4 exhibit similar conformations having twofold symmetry, while in 1 and 5 the anions exhibit C1 symmetry. The activity of the new compounds in the vulcanization of the natural rubber was evaluated and compared to the commercial accelerators ZDMC, TBBS and TMTD. These studies confirm that the sulfonyldithiocarbimato disulfides anions are new vulcanization accelerators, being slower than the commercial accelerators, but producing a greater degree of crosslinking, and scorch time values compatible with good processing safety for industrial applications. The mechanical properties, stress and tear resistances were determined and compared to those obtained with the commercial accelerators.

Crystal structure of the Hg4SiS6 and Hg4SiSe6 compounds

International Nuclear Information System (INIS)

Gulay, L.D.; Olekseyuk, I.D.; Parasyuk, O.V.

2002-01-01

The crystal structures of Hg 4 SiS 6 and Hg 4 SiSe 6 compounds were investigated using X-ray powder diffraction. These compounds crystallize in the monoclinic Cc space group with the lattice parameters a=1.23020(5), b=0.71031(4), c=1.22791(4) nm, β=109.721(3) deg. for Hg 4 SiS 6 and a=1.28110(4), b=0.74034(4), c=1.27471(1) nm, β=109.605(3) deg. for Hg 4 SiSe 6 . Atomic parameters were refined in the isotropic approximation (R I =0.0571 and R I =0.0555 for the Hg 4 SiS 6 and Hg 4 SiSe 6 , respectively)

Synthesis of Chalcone and Flavanone Compound Using Raw Material of Acetophenone and Benzaldehyde Derivative

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Ismiyarto Ismiyarto

2010-06-01

Full Text Available Synthesis of flavanoid compounds of chalcone and flavanone groups have been conducted. Flavanoid Is one of the group natural products which is mostly found in plants and have been proved to have physiological activity as drug. In this research, chalcone proup compounds that being synthesized are: chalcone, 3,4-dimethoxychalcone, 2'-hidroxy-3,4-dimethoxychalcone where as compound of flavanone group that being synthesized is 3',4'-dimethoxyflavanone. The synthesis of chalcone group are carried out based on Claisen-Schmidt reaction by using raw material of aromatic aldehydes and aromatic ketones. The synthesis in carried out by stirring at the room temperature using alkali solution as catalyst and ethanol as solvent. The synthesis of 3',4'-dimethoxyflanone is made based on the nucleophilic 1,4 addition of the unsaturated α,β ketone. The synthesis is made by refluxing 2'-hydroxy-3,4-dimethoxychalcone in alkali condition for 12 hours. The identification of flavanoid compound is carried out by using spectroscopic IR, GC-MS and 1H-NMR methods. The result of each synthesis chalcone group are follows: chalcone as yellowish solid with m.p= 50 °C and the yield is 83.39%; 3,4-dimethoxychalcone as yellow solid with m.p= 57°C and the yield is 76.00% ; 2'-hydroxy-3,4-dimethoxychalcone as orange solid with m.p= 90 °C and the yield is 74.29%, for 3',4'-dimethoxyflavanone as pale yellow solid with m.p= 80 °C and the yield is 72.00%.

Simple syntheses of 3-substituted indoles and their application for high yield 14C-labelling

International Nuclear Information System (INIS)

Schallenberg, J.; Meyer, E.

1983-01-01

Methods are described which allow the synthesis of several plant indole alkaloids and their metabolites at different scales. Compounds synthesized include gramine (1) (3-dimethylaminomethylindole) which is directly derived from indole, while its biosynthetic precursors 3-aminomethylindole (3) and 3-methylaminomethylindole (2) as well as indole3-carboxylic acid (7) are synthesized via indole-3-aldehyde (6). Slight changes of the experimental conditions allow syntheses with high yields not only at the molar but also at the μmolar level. This is extremely useful when isotope labelled compounds of high specific radioactivity are required for studies of plant metabolism. (orig.)

Antioxidant and DPPH (1,1-diphenyl-2-picrylhydrazyl Free Radical Scavenging Activities of New the Calix[4]arene-bodipy Derivative

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E. ERDEM

2014-07-01

Full Text Available p-tert-butylcalix[4]arene was synthesized with the condesation reaction of p-tert-butylphenol and formaldehyde in basic conditions and then has derivatized from the both of two hydroxyl position with chloride which is containing donor oxygen atoms. BODIPY compound (4,4-difluoro-4-bora-3a,4a-diaza-s-indacene was synthesized with appropriate pyrrole and aldehyde compounds and then was bonded p-tert-butylcalix[4]arene derivative via lower rim hydroxyl groups.The antioxidant activity of the calix[4]arene-BODIPY compound were determined using β-karotene-linoleic acid system. Moreover, the free radical scavenging activity values were tested with DPPH free radical. The compound showed strong antioxidant activity.Total antioxidant activity of the compound was determined using β–carotenelinoleic acid model system and was found the antioxidant activity of 72,50%. The free radical scavenging activities were determined as 75.19%. Results show that, calix[4]arene-BODIPY compound has the antioxidant activity. 

Synthesis and Characterization of the Rubidium Thiophosphate Rb 6 (PS 5 )(P 2 S 10 ) and the Rubidium Silver Thiophosphates Rb 2 AgPS 4 , RbAg 5 (PS 4 ) 2 and Rb 3 Ag 9 (PS 4 ) 4

KAUST Repository

Alahmary, Fatimah S.; Davaasuren, Bambar; Khanderi, Jayaprakash; Rothenberger, Alexander

2016-01-01

The metal thiophosphates Rb2AgPS4 (2), RbAg5(PS4)2 (3), and Rb3Ag9(PS4)4 (4) were synthesized by stoichiometric reactions, whereas Rb6(PS5)(P2S10) (1) was prepared with excess amount of sulfur. The compounds crystallize as follows: 1 monoclinic, P21

Two-dimensional inorganic–organic hybrid semiconductors composed of double-layered ZnS and monoamines with aromatic and heterocyclic aliphatic rings: Syntheses, structures, and properties

International Nuclear Information System (INIS)

Wang, Sujing; Li, Jing

2015-01-01

As an addition to the II–VI based inorganic–organic hybrid semiconductor family, five new two-dimensional (2D) double-layered structures have been synthesized employing monoamines with different aromatic or heterocyclic aliphatic rings. Zn 2 S 2 (bza) (1), Zn 2 S 2 (mbza) (2), Zn 2 S 2 (fbza) (3), Zn 2 S 2 (pca) (4), and Zn 2 S 2 (thfa) (5) (bza=benzylamine, mbza=4-methoxybenzylamine, fbza=4-flurobenzylamine, pca=3-picolylamine, and thfa=tetrahydrofurfurylamine) are prepared by solvothermal reactions and characterized by different analytical methods, including powder X-ray diffraction, optical diffuse reflection, thermogravimetric analysis and photoluminescence spectroscopy. The powder X-ray diffraction patterns show that all five compounds adopt 2D double-layered structures. Optical diffuse reflectance spectra of these compounds suggest that they have notably lower band gaps than those of the similar compounds composed of aliphatic alkyl amines. Their photoluminescence properties and thermal stability are also analyzed. - Graphical abstract: Five new members of two-dimensional double-layered 2D-Zn 2 S 2 (L) (L=Ligand) structures employing monoamines with different aromatic or heterocyclic aliphatic rings have been designed, synthesized, and characterized. - Highlights: • A new sub-family of II-VI based hybrid semiconductors are designed, synthesized, and structurally characterized using amines with aromatic or aliphatic cyclic rings. • These compounds have notably lower band gaps than those made of aliphatic alkyl amines, greatly broadening the range of band gaps of this material family. • They emit strongly with systematically tunable emission intensity and energy

Rapid detection of fluoride in potable water using a novel fluorogenic compound 7-O-tert-butyldiphenylsilyl-4-methylcoumarin

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Ravi Chavali

2015-12-01

Full Text Available In the present work, we have synthesized a new water soluble colorless chemical compound 7-O-tert-butyldiphenylsilyl-4-methylcoumarin (TBDPSC that releases fluorescent molecules imparting blue fluorescence to the solution, upon interaction with fluoride ions in water. The blue fluorescence can be visualized using simple hand held ultraviolet (UV lamps. TBDPSC has excellent sensitivity and selectivity towards fluoride and our results indicate that fluoride concentrations as low as 0.2 mg/L can be accurately detected within a few seconds. Fluoride testing with TBDPSC is simple and rapid compared to the conventional methodologies without the requirement of trained personnel. Hence, the present fluoride detection method can be easily field deployable and particularly useful for monitoring water quality in limited resource communities.

Ultrasound- and Molecular Sieves-Assisted Synthesis, Molecular Docking and Antifungal Evaluation of 5-(4-(Benzyloxy-substituted phenyl-3-((phenylaminomethyl-1,3,4-oxadiazole-2(3H-thiones

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Urja D. Nimbalkar

2016-05-01

Full Text Available A novel series of 5-(4-(benzyloxysubstituted phenyl-3-((phenyl aminomethyl-1,3,4-oxadiazole-2(3H-thione Mannich bases 6a–o were synthesized in good yield from the key compound 5-(4-(benzyloxyphenyl-1,3,4-oxadiazole-2(3H-thione by aminomethylation with paraformaldehyde and substituted amines using molecular sieves and sonication as green chemistry tools. The antifungal activity of the new products was evaluated against seven human pathogenic fungal strains, namely, Candida albicans ATCC 24433, Candida albicans ATCC 10231, Candida glabrata NCYC 388, Cryptococcus neoformans ATCC 34664, Cryptococcus neoformans PRL 518, Aspergillus fumigatus NCIM 902 and Aspergillus niger ATCC 10578. The synthesized compounds 6d, 6f, 6g, 6h and 6j exhibited promising antifungal activity against the tested fungal pathogens. In molecular docking studies, derivatives 6c, 6f and 6i showed good binding at the active site of C. albicans cytochrome P450 enzyme lanosterol 14 α-demethylase. The in vitro antifungal activity results and docking studies indicated that the synthesized compounds have potential antifungal activity and can be further optimized as privileged scaffolds to design and develop potent antifungal drugs.

Antibacterial potential of silver nanoparticle synthesized by marine ...

African Journals Online (AJOL)

Multi resistance to antibiotics is a serious and disseminated clinical problem, common to several new compounds that block the resistance mechanism. The present study aimed at the comparative study of silver nanoparticles synthesized through actinomycetes and their antimicrobial metabolites with standard antibiotic.

1-[3-(2-Methyl-4-phenylquinolin-3-yl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]-propane-1-one

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Allaoua Kedjadja

2015-06-01

Full Text Available A novel compound, 1-[3-(2-methyl-4-phenylquinolin-3-yl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]-propane-1-one (3 has been synthesized by cyclocondensation of (E-1-(2-methyl-4-phenylquinolin-3-yl-3-phenylprop-2-en-1-one (2 and hydrazine hydrate in propionic acid. The structure of this compound was established by elemental analysis, IR, 1H-NMR, 13C-NMR and MS data.

Influence of annealing temperature on the electrochemical and surface properties of the 5-V spinel cathode material LiCr0.2Ni0.4Mn1.4O4 synthesized by a sol–gel technique

DEFF Research Database (Denmark)

Younesi, Reza; Malmgren, Sara; Edström, Kristina

2014-01-01

LiCr0.2Ni0.4Mn1.4O4 was synthesized by a sol–gel technique in which tartaric acid was used as oxide precursor. The synthesized powder was annealed at five different temperatures from 600 to 1,000 °C and tested as a 5-V cathode material in Li-ion batteries. The study shows that annealing at higher...

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

Science.gov (United States)

Qian, Cheng; Kong, Fang; Mao, Jiang-Gao

2016-06-01

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy)2V2O4(SeO3)2 (1), Cu(2,2-bipy)V2O4(SeO3)2·0.5H2O (2) and Cu2(2,2-bipy)2V5O12(SeO3)2 (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy)2V2O4(SeO3)2}2 dimeric cluster composed of two {Ni(2,2-bipy)2}2+ moieties connected by the {V4O8(SeO3)4}4- cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V2O4(SeO3)2}n chain in which the {Cu2(2,2-bipy)2}4+ moieties are bridged by the {V4O8(SeO3)4}4- clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {VIVVV4SeIV2O18}n4- and {Cu(2,2-bipy)}2+ complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V4O8(SeO3)4}4- cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties.

Syntheses and in Vitro Antiplasmodial Activity of Aminoalkylated Chalcones and Analogues.

Science.gov (United States)

Wilhelm, Anke; Kendrekar, Pravin; Noreljaleel, Anwar E M; Abay, Efrem T; Bonnet, Susan L; Wiesner, Lubbe; de Kock, Carmen; Swart, Kenneth J; van der Westhuizen, Jan Hendrik

2015-08-28

A series of readily synthesized and inexpensive aminoalkylated chalcones and diarylpropane analogues (1-55) were synthesized and tested against chloroquinone-sensitive (D10 and NF54) and -resistant (Dd2 and K1) strains of Plasmodium falciparum. Hydrogenation of the enone to a diarylpropane moiety increased antiplasmodial bioactivity significantly. The influence of the structure of the amine moiety, A-ring substituents, propyl vs ethyl linker, and chloride salt formation on further enhancing antiplasmodial activity was investigated. Several compounds have IC₅₀ values similar to or better than chloroquine (CQ). The most active compound (26) had an IC₅₀ value of 0.01 μM. No signs of resistance were detected, as can be expected from compounds with structures unrelated to CQ and other currently used antimalarial drugs. Toxicity tests (in vitro CHO cell assay) gave high SI indices.

A novel inorganic-organic compound: Synthesis and structural characterization of tin(II) phenylbis(phosphonate), Sn2(PO3C6H4PO3)

International Nuclear Information System (INIS)

Subbiah, Ayyappan; Bhuvanesh, Nattamai; Clearfield, Abraham

2005-01-01

A novel tin(II) phenylbis(phosphonate) compound has been synthesized hydrothermally and its structure has been determined by single crystal X-ray diffraction. The structure is monoclinic, space group P2 1 /c (no. 14), a=4.8094(4), b=16.2871(13), c=6.9107(6)A; β=106.292(6) o , V=519.59(7)A 3 , Z=2. The three-dimensional structure consists of 3-coordinated tin and 4-coordinated phosphorus double layers separated (pillared) by phenyl rings. These phenyl rings are placed 4.8A apart along the a-axis in the structure resulting in lower surface area (∼14m 2 /g). The porosity has been increased by replacing phenyl groups by methyl groups (∼31m 2 /g)

Hydrothermal synthesis of layered iron-chalcogenide superconductors and related compounds

International Nuclear Information System (INIS)

Pachmayr, Ursula Elisabeth

2017-01-01

This thesis provides a new preparative approach to iron-chalcogenide based superconductors. The hydrothermal synthesis of anti-PbO type FeSe, which can be seen as basis structure of the compounds of interest was successfully developed. Along with this, some insights regarding the influence of synthesis parameters were gained featuring a basis for further hydrothermal syntheses of new iron-chalcogenide compounds. The potential of this method, primarily the extension of the so far limited accessibility of iron-chalcogenide based superconductors by solid-state sythesis, was revealed within the present work. The solid-solution FeSe_1_-_xS_x was prepared for the whole substitution range, whereas solid-state synthesis exhibits a solubility limit at x = 0.3. Furthermore, the new compounds [(Li_0_._8Fe_0_._2)OH]FeX (X = Se, S) were synthesized which are exclusively accessible via hydrothermal method. The compounds, where layers of (Li_0_._8Fe_0_._2)OH alternate with FeX layers, feature exceptional physical properties, notably a coexistence of superconductivity and ferromagnetism. They were intensively studied within this work. By combination of solid-state and hydrothermal ion-exchange synthesis even large crystals necessary for subsequent physical measurements are accessible. Apart from these layered iron-chalcogenide superconductors, further compounds which likewise exhibit building blocks of edge-sharing FeSe_4 tetrahedra were found via this synthesis method. The iron selenides A_2Fe_4Se_6 (A = K, Rb, Cs) consist of double chains of [Fe_2Se_3]"1"-, whereas a new compound Na_6(H_2O)_1_8Fe_4Se_8 exhibits [Fe_4Se_8]"6"- 'stella quadrangula' clusters. This structural diversity as well as the associated physical properties of the compounds demonstrates the numerous capabilities of hydrothermal synthesis in the field of iron-chalcogenide compounds. In particular with regard to iron-chalcogenide based superconductors this synthesis strategy is encouraging. It seems probable

Hydrothermal synthesis of layered iron-chalcogenide superconductors and related compounds

Energy Technology Data Exchange (ETDEWEB)

Pachmayr, Ursula Elisabeth

2017-04-06

This thesis provides a new preparative approach to iron-chalcogenide based superconductors. The hydrothermal synthesis of anti-PbO type FeSe, which can be seen as basis structure of the compounds of interest was successfully developed. Along with this, some insights regarding the influence of synthesis parameters were gained featuring a basis for further hydrothermal syntheses of new iron-chalcogenide compounds. The potential of this method, primarily the extension of the so far limited accessibility of iron-chalcogenide based superconductors by solid-state sythesis, was revealed within the present work. The solid-solution FeSe{sub 1-x}S{sub x} was prepared for the whole substitution range, whereas solid-state synthesis exhibits a solubility limit at x = 0.3. Furthermore, the new compounds [(Li{sub 0.8}Fe{sub 0.2})OH]FeX (X = Se, S) were synthesized which are exclusively accessible via hydrothermal method. The compounds, where layers of (Li{sub 0.8}Fe{sub 0.2})OH alternate with FeX layers, feature exceptional physical properties, notably a coexistence of superconductivity and ferromagnetism. They were intensively studied within this work. By combination of solid-state and hydrothermal ion-exchange synthesis even large crystals necessary for subsequent physical measurements are accessible. Apart from these layered iron-chalcogenide superconductors, further compounds which likewise exhibit building blocks of edge-sharing FeSe{sub 4} tetrahedra were found via this synthesis method. The iron selenides A{sub 2}Fe{sub 4}Se{sub 6} (A = K, Rb, Cs) consist of double chains of [Fe{sub 2}Se{sub 3}]{sup 1-}, whereas a new compound Na{sub 6}(H{sub 2}O){sub 18}Fe{sub 4}Se{sub 8} exhibits [Fe{sub 4}Se{sub 8}]{sup 6-} 'stella quadrangula' clusters. This structural diversity as well as the associated physical properties of the compounds demonstrates the numerous capabilities of hydrothermal synthesis in the field of iron-chalcogenide compounds. In particular with regard

Three new Ag(I) coordination architectures based on mixed ligands: Syntheses, structures and photoluminescent properties

Energy Technology Data Exchange (ETDEWEB)

Li, Yamin, E-mail: liyamin@henu.edu.cn [Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Xiao, Changyu; Li, Shu; Chen, Qi; Li, Beibei; Liao, Qian; Niu, Jingyang [Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China)

2013-04-15

Three new silver (I) coordination complexes, [Ag{sub 2}(1,2-bdc)(phdat)]{sub n} (1), [Ag{sub 2}(NO{sub 2}-bdc)(phdat)]{sub n} (2), [Ag{sub 4}(nta){sub 3}(phdat)NO{sub 3}]{sub n} (3) (1,2-bdc=phthalic acid dianion, NO{sub 2}-bdc=5-nitro-1,3-benzenedicarboxylic acid dianion, nta=nicotinic acid anion, phdat=2,4-diamine-6-phenyl-1,3,5-triazine) have been hydrothermally synthesized by the reactions of silver nitrate and phdat with the homologous ligands 1,2-H{sub 2}bdc, NO{sub 2}-H{sub 2}bdc, and Hnta, respectively, and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses thermogravimetric analyses (TGA). The compound 1 exhibits a chiral 3D network with cbs/CrB self-dual topological net, which contains two kinds of single helical chains. For compound 2, the 3D network is comprised of two kinds of similar 2D sheets with the topological symbol of sql-type packed in AABBAA mode by Ag–N/O weakly contacts. And compound 3 has 2D double layer architecture, consisting of the 2D plane with hcb-type topological symbol connected by Ag–O weakly coordinations. The photoluminescent properties associated with the crystal structures of three compounds have also been measured. - Graphical abstract: Three new silver(I) coordination complexes 1–3 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses (TGA) and photoluminescent spectra. Highlights: ► The compound 1 exhibits a novel chiral 3D network with two kinds of single helical chains. ► 3D or 2D new Ag coordination complexes. ► The photoluminescent properties have been measured.

Synthesis of the compound tetrakis (2- methoxy isobutyl isonitrile) copper (I) tetrafluoroborate -(Cu[MIBI]4BF4): substance used in the production of the radiopharmaceutical sestamibi 99m Tc

International Nuclear Information System (INIS)

Silva, Katia Suzi da Silveira

2005-01-01

The radiopharmaceutical SESTAMIBI- 99m Tc presents interest and application in the clinical routine in Nuclear Medicine, especially for evaluation of the myocardium function and in the diagnosis of some tumors types, and the Center of Radiopharmacy of the IPEN has interest in the development of this radiopharmaceutical for attendance of the nuclear medicine class necessities. In this work it was demonstrated the synthesis and characterization of the active compound tetrakis (2- methoxy isobutyl isonitrile) copper (I) tetrafluoroborate - Cu[MIBI] 4 BF 4 - to be used in the preparation of lyophilized reagents for labeling with technetium- 99m as well as labeling studies and biological distribution. The synthesis of the reagent Cu[MIBI] 4 BF 4 was carried out in accordance with previously described procedures, in 5 steps and the compounds were characterized for infra-red, magnetic nuclear resonance, melting point and thin layer chromatography. The characterization of the chelate of MIBI -Cu[MIBI] 4 BF 4 - was carried out using high performance liquid chromatography, compared with a standard sample of the product and presented similar results, as described in literature. The lyophilized reagent was prepared and labeled with technetium- 99m , showing high radiochemical purity, higher than 97%, with high stability. Biological distribution in different animals showed good uptake in the heart, in time compatible with the acquisition of scintigraphy images, demonstrating the applicability of the reagent synthesized in the attainment of cardiac scintigraphy images. (author)

Naturally Abundance Vanillin as Starting Material to Synthesizing 4-(4-Hydroxy-3-methoxyphenyl-6-methyl-3,4-dihydropyrimidin-2(1H-one

Directory of Open Access Journals (Sweden)

Masruri MASRURI

2015-12-01

Full Text Available Indonesia is the second biggest producer of natural vanillin. Traditionally it was isolated from the bean of vanilla (Vanilla planifolia Andrews. This paper reports on applying vanillin as starting material for synthesizing a biologically important chemical structure 3,4-dihydropyrimidinone. The reaction was undertaken in one step following multi component reaction (MCR. Products determination was undergone using FTIR and UV-Vis spectrophotometry, and also liquid chromatography-mass spectrometry (LCMS. After purification under flash column chromatography in ethyl acetate-hexane, it was found a white solid of 4-(4-hydroxy-3-methoxyphenyl-6-methyl-3,4-dihydropyrimidin-2(1H-one in 67% yield with a few amount of an unreacted vanillin.

Synthesis of chiral pyrazolo[4,3-e][1,2,4]triazine sulfonamides with tyrosinase and urease inhibitory activity.

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Mojzych, Mariusz; Tarasiuk, Paweł; Kotwica-Mojzych, Katarzyna; Rafiq, Muhammad; Seo, Sung-Yum; Nicewicz, Michał; Fornal, Emilia

2017-12-01

A new series of sulfonamide derivatives of pyrazolo[4,3-e][1,2,4]triazine with chiral amino group has been synthesized and characterized. The compounds were tested for their tyrosinase and urease inhibitory activity. Evaluation of prepared derivatives demonstrated that compounds (8b) and (8j) are most potent mushroom tyrosinase inhibitors whereas all of the obtained compounds showed higher urease inhibitory activity than the standard thiourea. The compounds (8a), (8f) and (8i) exhibited excellent enzyme inhibitory activity with IC 50 0.037, 0.044 and 0.042 μM, respectively, while IC 50 of thiourea is 20.9 μM.

Coordination compounds of cobalt and cadmium with isobutyric acid amide

International Nuclear Information System (INIS)

Tsivadze, A.Yu.; Ivanova, I.S.; Solovkina, O.A.

1983-01-01

Coordination compounds of cobalt and cadmium with isobutyric acid amide (IBAA) of Co(NCS) 2 x(IBAA) 2 (H 2 O) 2 , CoCl 2 (IBAA) 4 , CoI 2 (IBAA) 8 (H 2 O) 2 , CdI 2 (IBAA) 2 composition have been synthesized and characterized. Their infrared absorption spectra (200-400 cm -1 ), electron reflection spectra (200-750 nm) were studied. It is shown that in all compounds there are IBAA molecUles coordinated through an oxygen atom. Thiocyanogroups are coordinated throUgh nitrogen atoms

Exploiting the pyrazolo[3,4-d]pyrimidin-4-one ring system as a useful template to obtain potent adenosine deaminase inhibitors.

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La Motta, Concettina; Sartini, Stefania; Mugnaini, Laura; Salerno, Silvia; Simorini, Francesca; Taliani, Sabrina; Marini, Anna Maria; Da Settimo, Federico; Lavecchia, Antonio; Novellino, Ettore; Antonioli, Luca; Fornai, Matteo; Blandizzi, Corrado; Del Tacca, Mario

2009-03-26

A number of pyrazolo[3,4-d]pyrimidin-4-ones bearing either alkyl or arylalkyl substituents in position 2 of the nucleus were synthesized and tested for their ability to inhibit adenosine deaminase (ADA) from bovine spleen. The 2-arylalkyl derivatives exhibited excellent inhibitory activity, showing Ki values in the nanomolar/subnanomolar range. The most active compound, 1-(4-((4-oxo-4,5-dihydropyrazolo[3,4-d]pyrimidin-2-yl)methyl)phenyl)-3-(4-(trifluoromethyl)phenyl)urea, 14d, was tested in rats with colitis induced by 2,4-dinitrobenzenesulfonic acid to assess its efficacy to attenuate bowel inflammation. The treatment with 14d induced a significant amelioration of both systemic and intestinal inflammatory alterations in animals with experimental colitis. Docking simulations of the synthesized compounds into the ADA catalytic site were also performed to rationalize the structure-activity relationships observed and to highlight the key pharmacophoric elements of these products, thus prospectively guiding the design of novel ADA inhibitors.

Syntheses, structures and third-order non-linear optical properties of homometal clusters containing molybdenum

International Nuclear Information System (INIS)

Li Yong; Lu Jing; Cui Xiaobing; Xu Jiqing; Li Kechang; Sun Huaying; Li Guanghua; Pan Lingyun; Yang Qingxin

2005-01-01

Both the homometal cluster [P(ph 4 )] 2 [Mo 2 O 2 (μ-S) 2 (S 2 ) 2 ] (1) and [Mo 2 O 2 (μ-S) 2 (Et 2 dtc) 2 ] (2) (Et 2 dtc=diethyl-dithiocarbamate) were successfully synthesized by low-temperature solid-state reactions. X-ray single-crystal diffraction studies suggest that compound (1) is a dinuclear anion cluster, and compound (2) is a dinuclear neutral cluster. The two compounds were characterized by elemental analyses, IR spectra and UV-Vis spectra. The third-order non-linear optical (NLO) properties of the clusters were also investigated and all exhibited nice non-linear absorption and self-defocusing performance with moduli of the hyperpolarizabilities 5.145x10 -30 esu for (1) and 5.428x10 -30 esu for (2)

Rh(III)-Catalyzed C-H Activation of Benzoylacetonitriles and Tandem Cyclization with Diazo Compounds to Substituted Benzo[ de]chromenes.

Science.gov (United States)

Fang, Feifei; Zhang, Chunmei; Zhou, Chaofan; Li, Yazhou; Zhou, Yu; Liu, Hong

2018-04-06

Rh (III)-catalyzed C-H activation of benzoylacetonitriles in coupling with diazo compounds was developed to synthesize diversified substituted benzo[ de]chromenes via a formal (4 + 2) cycloaddition with a diazo compound and subsequent tandem (4 + 2) cycloaddition with another diazo compound. Intriguingly, synthesis of substituted benzo[ de]chromenes and their decarboxylation products could be realized by controlling the reaction conditions. These reactions have a broad range of substrates, moderate to good yields, and high regioselectivity.

New hydride compounds of 1,4-diazabicyclo[2.2.2]octane and its dication with borine and tetrahydridoborate anion and products of their transformations; Novye gidridnye soedineniya 1,4-diazabitsiklo[2.2.2]oktana i ego dikationa s borinom i tetergidridoborat-anionom i produkty ikh prevrashcheniya

Energy Technology Data Exchange (ETDEWEB)

Shevchenko, Yu N; Yashina, N I; Markova, O Z; Trachevskij, V V

1997-12-31

New compounds [dabcoH{sub 2}](BH{sub 4}){sub 2}, dabco(BH{sub 3}){sub 2}2H{sub 2}, [dabco(BH{sub 3}){sub 2}H{sub 2}]{sub n} have been synthesized by means of interaction between dihydrochloride of 1,4-diazobicyclo[2.2.2] octane (dabco) and NaBH{sub 4} in the medium of nonaqueous solvents (glyme, diglyme, tetrahydrofuran, dimethylsulfoxide) and identified by the methods of element analysis, conductometry, {sup 1}H, {sup 11}B, {sup 14}N NMR, IR spectroscopy and thermal analysis. A mechanism is suggested and the conditions are defined for mutual transformations of the compounds studied. Their ability to bind reversibly molecular hydrogen has been revealed for the first time. 19 refs.; 3 figs.; 1 tab.

Ruthenium(II carbonyl compounds with the 4′-chloro-2,2′:6′,2′′-terpyridine ligand

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Rajendhraprasad Tatikonda

2017-04-01

Full Text Available Two ruthenium carbonyl complexes with the 4′-chloro-2,2′:6′,2′′-terpyridine ligand (tpy-Cl, C15H10ClN3, i.e. [RuCl(tpy-Cl(CO2][RuCl3(CO3] (I [systematic name: cis-dicarbonylchlorido(4′-chloro-2,2′:6′,2′′-terpyridine-κ3Nruthenium(II fac-tricarbonyltrichloridoruthenate(II], and [RuCl2(tpy-Cl(CO2] (II [cis-dicarbonyl-trans-dichlorido(4′-chloro-2,2′:6′,2′′-terpyridine-κ2N1,N1′ruthenium(II], were synthesized and characterized by single-crystal X-ray diffraction. The RuII atoms in both centrosymmetric structures (I and (II display similar, slightly distorted octahedral coordination spheres. The coordination sphere in the complex cation in compound (I is defined by three N atoms of the tridentate tpy-Cl ligand, two carbonyl carbon atoms and one chlorido ligand; the charge is balanced by an octahedral [Ru(CO3Cl3]− counter-anion. In the neutral compound (II, the tpy-Cl ligand coordinates to the metal only through two of its N atoms. The coordination sphere of the RuII atom is completed by two carbonyl and two chlorido ligands. In the crystal structures of both (I and (II, weak C—H...Cl interactions are observed.

1,1′-{1,4-Phenylene bis[3-(6-chloro-2-methyl-4-phenylquinolin-3-yl-4,5-dihydro-1H-pyrazole-5,1-diyl]}dibutan-1-one

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Allaoua Kedjadja

2015-10-01

Full Text Available A new polycyclic compound, 1,1′-{1,4-phenylene bis[3-(6-chloro-2-methyl-4-phenylquinolin-3-yl-4,5-dihydro-1H-pyrazole-5,1-diyl]}dibutan-1-one (3 has been synthesized by cyclocondensation of (2E,2′E-1,1′-bis(6-chloro-2-methyl-4-phenylquinolin-3-yl-3,3′-(1,4-phenylenediprop-2-en-1-one (2 and hydrazine hydrate in butanoic acid. The structure of this compound was established by elemental analysis, 1H-NMR, 13C-NMR, mass and IR spectroscopy.

Microalgae associated Brevundimonas sp. MSK 4 as the nano particle synthesizing unit to produce antimicrobial silver nanoparticles.

Science.gov (United States)

Rajamanickam, Karthic; Sudha, S S; Francis, Mebin; Sowmya, T; Rengaramanujam, J; Sivalingam, Periyasamy; Prabakar, Kandasamy

2013-09-01

The biosynthesis of silver nanoparticles and its antimicrobial property was studied using bacteria isolated from Spirulina products. Isolated bacteria were identified as Bacillus sp. MSK 1 (JX495945), Staphylococcus sp. MSK 2 (JX495946), Bacillus sp. MSK 3 (JX495947) and Brevundimonas sp. MSK 4 (JX495948). Silver nanoparticles (AgNPs) were synthesized using bacterial culture filtrate with AgNO3. The initial syntheses of Ag nanoparticles were characterized by UV-vis spectrophotometer (by measuring the color change to intense brown). Fourier Transform Infrared Spectroscopy (FTIR) study showed evidence that proteins are possible reducing agents and Energy-dispersive X-ray (EDX) study showing the metal silver as major signal. The structure of AgNPs was determined by Scanning electron microscopy (SEM) and X-ray diffraction (XRD). Synthesized Ag nanoparticles with an average size of 40-65 nm have antimicrobial property against human pathogens like Proteus vulgaris, Salmonella typhi, Vibrio cholera, Streptococcus sp., Bacillus subtilis, Staphylococcus aureus, and Escherichia coli. Among the isolates Brevundimonas sp. MSK 4 alone showed good activity in both synthesis of AgNPs and antimicrobial activity. This work demonstrates the possible use of biological synthesized silver nanoparticles to combat the drug resistant problem. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and biological activity of n-{5-(4-methylphenyl diazenyl-4-phenyl-1, 3-thiazol-2-yl}benzamide derivatives

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Ashishkumar Kantilal Prajapati

2011-01-01

Full Text Available In the present study, various amides of 2-amino-5-(4-methylphenyl-diazenyl-4-phenyl-1, 3-thiazole was synthesized and their biological activities were evaluated. All the synthesized compounds were characterized by the combination of elemental analysis and standard spectroscopic methods. They are screened for anti-bacterial activity against Escherichia coli and Staphylococcus aureus as well as screened for antifungal activity against Aspergillus niger and Apergillus oryzae by cup plate method at 1 µg/ mL concentration in DMF.

Synthesis and biological activity of N-{5-(4-methylphenyl) diazenyl-4-phenyl-1, 3-thiazole-2-yl}benzamide derivatives

International Nuclear Information System (INIS)

Prajapati, Ashishkumar K.; Modi, Vishal P.

2011-01-01

In the present study, various amides of 2-amino-5-(4-methylphenyl)-diazenyl-4-phenyl-1, 3-thiazole was synthesized and their biological activities were evaluated. All the synthesized compounds were characterized by the combination of elemental analysis and standard spectroscopic methods. They are screened for anti-bacterial activity against Escherichia coli and Staphylococcus aureus as well as screened for antifungal activity against Aspergillus niger and Aspergillus oryzae by cup plate method at 1 μg/ mL concentration in DMF. (author)

SYNTHESIS, CHARACTERIZATION AND ANTI-BACTERIAL ACTIVITY OF CERTAIN 2,3,4,5-TETRAHYDROPYRIDAZINONE ANALOGUES

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Gaurav ALANG

2011-04-01

Full Text Available In the present study, six new derivatives of PYridazinone were synthesized and evaluate their anti-bacterial activity. The experimental work involves the synthesis of benzoyl propionic acid (a, then 6-phenyl-2,3,4,5-tetrahydro pyridazin-3-one (b which was then condensed with various, aldehydes to form respective derivatives, AH the synthesized compounds were identified by IR, 1HNMR and antimicrobial activity was performed on the compounds synthesized against Staphylococcus aureus (MTCC 737, Staphylococcus epidermidis (MTCC 3615, Pseudomonas aeruginosa (MTCC 424 and Escherichia coli (MTCC 1687

5-Methyl-3,8-di-(2-amino-4-bromophenyl-4,9-dioxa-1,2,6,7-tetraaza-5λ5-phosphaspiro[4.4]nona-2,7-diene

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Sławomir Kasperowicz

2018-01-01

Full Text Available 5-Methyl-3,8-di-(2-amino-4-bromophenyl-4,9-dioxa-1,2,6,7-tetraaza-5λ5-phosphaspiro[4.4]nona-2,7-diene was obtained by condensation of 2-amino-5-bromobenzohydrazide and methylphosphonyl dichloride in the presence of triethylamine. An initial biological screening was performed for the resulting product. The synthesized compound showed relatively strong cytotoxic activity, which was, however, similar for cancer and non-cancer cell lines.

A new class of potential chloroquine-resistance reversal agents for Plasmodia: syntheses and biological evaluation of 1-(3'-diethylaminopropyl)-3-(substituted phenylmethylene)pyrrolidines.

Science.gov (United States)

Batra, S; Srivastava, P; Roy, K; Pandey, V C; Bhaduri, A P

2000-09-07

1-(3'-Diethylaminopropyl)-3-(substituted phenylmethylene)pyrrolidines were synthesized and evaluated for CQ-resistant reversal activity. In general the compounds of the series elicit better biological response than their phenylmethyl analogues. The most active compound 4b has been evaluated in vivo in detail, and the results are presented. The possible mode of action of the compounds of this series is by inhibition of the enzyme heme oxygenase, thereby increasing the levels of heme and hemozoin, which are lethal to the parasite.

Syntheses of 4-aminobutanoic acid-2,2-/sup 2/H/sub 2/ and -4,4-/sup 2/H/sub 2/ and progabide-2,2-/sup 2/H/sub 2/ and -4,4-/sup 2/H/sub 2/

Energy Technology Data Exchange (ETDEWEB)

Davis, B.

1987-10-01

4-Aminobutanoic acid-2,2-/sup 2/H/sub 2/ and -4,4-/sup 2/H/sub 2/ were synthesized in high yield with high deuterium incorporation, and then converted into the corresponding deuterium-labelled anti-convulsant drug, progabide, by means of a transimination reaction.

Infrared spectroscopy of some organocobalt (III) compounds

International Nuclear Information System (INIS)

Benedetti, A.V.; Mauro, A.E.

1982-01-01

The compounds [MeCo(DH) 2 py], [MeCo(DH) 2 H 2 O] (M = methyl; DH = dimethyl-glyoxymate; py = pyridine) and others of general formulae [Co(L)(H 2 O) 2 ] ClO 4 , where L = SALOPHEN = bis (salicylaldehyde)-o-phenylenediimine; SALCN = 1,2-bis (salicylaldehyde) cyclohexylenediimine; SALEN = bis (salicylaldehyde) ethylenediimine; BAE = bis (acetylacetone)-ethylenediimine were synthesized and studied by infrared spectroscopy. The frequencies observed have been assigned to specific group vibrations. (Author) [pt

Synthesis, crystal structures, computational studies and antimicrobial activity of new designed bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes

Science.gov (United States)

Ahmed, Muhammad Naeem; Sadiq, Beenish; Al-Masoudi, Najim A.; Yasin, Khawaja Ansar; Hameed, Shahid; Mahmood, Tariq; Ayub, Khurshid; Tahir, Muhammad Nawaz

2018-03-01

A new series of bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes 4-14 have been synthesized via nucleophilic substitution reaction of dihaloalkanes with respective 1,3,4-oxadiazole-2-thiols 3a-f, and characterized by spectroscopic techniques. The structures of 4 and 12 were unambiguously confirmed by single-crystal X-ray diffraction analysis. Density functional theory calculations at B3LYP/6-31 + G(d) level of theory were performed for comparison of X-ray geometric parameters, molecular electrostatic potential (MEP) and frontier molecular orbital analyses of synthesized compounds. MEP analysis revealed that these compounds are nucleophilic in nature. Frontier molecular orbitals (FMOs) analysis of 4-14 was performed for evaluation of kinetic stability. All synthesized compounds were screened in vitro for antimicrobial activity against three bacterial and three fungal strains and showed promising results.

Synthesis and anti-lung cancer activity of a novel arsenomolybdate compound

Science.gov (United States)

Zhu, Tian-Tian; Wang, Juan; Chen, Song-Hu

2017-12-01

The new compound based on Wells-Dawson-type arsenomolybdate: [{Cu10(pz)11Cl4}{As2IIIAs2VMo6VMo12VIO62}]·H2O (1) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis, X-ray powder diffraction (XRPD), XPS spectroscopy and thermogravimetric analysis (TG). Compound 1 is consisted of two As caps Wells-dawson-type arsenomolybdate and {Cu10(py)11} complexes by chloride bridge. In addition, the antitumor effects of the title compound 1 were studied on three human lung cancer cells (A549, SK-LU-1 and SW1573). The results showed that compared with the positive reference drug carboplatin, compound 1 displayed efficient antitumor activity.

Iron based superconductors and related compounds synthesized by solid state metathesis and high temperature reactions

International Nuclear Information System (INIS)

Frankovsky, Rainer

2013-01-01

The results of this thesis can be divided into three major topics, which can also be seen as different approaches of solid state chemistry to reveal interesting features of known and unknown compounds and to develop alternative synthesis routes. Firstly, known compounds with related structural motifs to the superconducting iron-arsenides were investigated regarding their structural and physical properties. In case of La 3 Pd 4 Ge 4 the influence of Fe doping on the properties was studied, whereas in the series ZrMAs (M=Ti,V) the physical properties have not yet been reported at all and were investigated for the first time. Secondly, an alternative synthesis route has been developed for the synthesis of superconducting LaFeAsO 1-x F x . This solid state metathesis reaction distinctly increased the quality of the samples compared to conventionally prepared products. Furthermore, the reaction pathway was investigated and clarified, which helps to understand the processes during high temperature solid state metathesis reactions in general. Thirdly, this alternative synthesis route was expanded to other systems and new compounds like co-substituted LaFe 1-x Mn x AsO 1-y F y were prepared and thoroughly investigated. This led to a complex study of the interplay of magnetism, electronic and structural conditions and the occurrence of superconducting properties. The investigation and understanding of such complex coherences will probably be decisive for the further understanding of the superconducting mechanism in iron based superconductors.

Electroactive chain-like compounds constructed from trimetallic clusters and 4,4'-bipyridine spacers: one-pot synthesis, characterization and surface binding.

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Abe, Masaaki; Inatomi, Atsushi; Hisaeda, Yoshio

2011-03-14

This paper reports the synthesis and characterization of a novel series of chain-like compounds where oxo-centered triruthenium cluster moieties are bridged by 4,4'-bipyridine (4,4'-bpy) spacers. A reaction of solvent-coordinated triruthenium "monomer" precursor [Ru(3)O(CH(3)CO(2))(6)(CO)(CH(3)OH)(2)] with a 0.1 equimolar amount of 4,4'-bpy in CH(3)OH gave mixture of chain-like compounds containing "dimers" to "tetramers" which were cleanly separated by column chromatography and characterized by spectroscopic and electrochemical methods. Cyclic voltammetry revealed that all chain-like compounds exhibit reversible and stepwise redox processes in solution with very weak intramolecular coupling between the triruthenium components across the 4,4'-bpy bridge. Photo-induced dissociation of CO from the compounds and electrode surface binding were also investigated.

Novel Schiff Bases Based on the Quinolinone Skeleton: Syntheses, X-ray Structures and Fluorescent Properties

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Zdeněk Trávníček

2014-09-01

Full Text Available A series of a new type of Schiff bases 1–7, derived from 2-phenyl-3-amino-4(1H-quinolinone and R-salicyladehyde derivatives wherein R = 3-hydroxy (1, 3,4-dihydroxy (2, 3-methoxy (3, 3-carboxy (4, 3-allyl (5, 5-chloro (6, and 5-nitro (7, was synthesized and structurally characterized. Each of the molecules 1, 3 and 7 consists of three planar moieties (i.e., a quinolinone and two phenyl rings, which are mutually oriented differently depending on the appropriate substituent R and the extent of non-covalent contacts stabilizing the crystal structures. The compounds were studied for their fluorescence properties, where compound 6 yielded the strongest intensity both in the solid phase and in 100 μM ethanol solution with a quantum yield of φ = 3.6% as compared to quinine sulfate used as a standard. The in vitro cytotoxicity of these compounds was tested against the human osteosarcoma (HOS and breast adenocarcinoma (MCF7 cell lines, revealing no activity up to the concentration of 50 µM.

Synthesis of schiff bases of pyridine-4-carbaldehyde and their antioxidant and DNA binding studies

International Nuclear Information System (INIS)

Shamim, S.; Murtaza, S.; Nazar, M.F.

2016-01-01

A series of Schiff bases of pyridine-4-carbaldehyde with 3-aminobenzoic acid, 2-aminobenzoic acid, 4-aminobenzoic acid, 1,3-phenylenediamine, 1,2-phenylenediamine, 2-aminothiophenol, 4-aminoantipyrene, 2-aminophenol and naphthalene-1-amine was synthesized and compounds were characterized by FTIR, NMR and mass spectrometry. The synthesized compounds were evaluated for their antioxidant and DNA binding interaction studies. DPPH scavenging method was used to evaluate the antioxidant activities of synthesized Schiff bases at six gradually increasing concentrations of 0.5-5mg/ml. 2-((pyridin-4-ylmethylidene)amino)phenol came out to be the most efficient antioxidant at a concentration of 4mg/ml with 74% inhibition of free radicals generated by DPPH. The DNA binding interaction of the synthesized Schiff bases was determined using UV-Vis absorption titration method. Both the hypochromic and hyperchromic effects were observed along the series. The values for the binding constant (K) and free energy change (G) were calculated and most of the Schiff bases have high positive K values which indicate the efficient binding of Schiff bases with DNA. Molecular docking studies as carried out using PatchDock molecular algorithm software also indicated the high values for geometrical shape complementarity score suggesting the stabilities of Schiff bases/DNA complex. Docking studies also suggested the minor groove binding of the Schiff bases with DNA. Drug-likeness of the synthesized compounds was also tested in silico and the results are accordingly discussed. (author)

A series of 2D metal-quinolone complexes: Syntheses, structures, and physical properties

Energy Technology Data Exchange (ETDEWEB)

He, Jiang-Hong [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Xiao, Dong-Rong, E-mail: xiaodr98@yahoo.com.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Chen, Hai-Yan; Sun, Dian-Zhen; Yan, Shi-Wei; Wang, Xin; Ye, Zhong-Li [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Luo, Qun-Li, E-mail: qlluo@swu.edu.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Wang, En-Bo, E-mail: wangeb889@nenu.edu.cn [Key Laboratory of Polyoxometalate Science of Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun 130024 (China)

2013-02-15

Six novel 2D metal-quinolone complexes, namely [Cd(cfH)(bpdc)]{center_dot}H{sub 2}O (1), [M(norfH)(bpdc)]{center_dot}H{sub 2}O (M=Cd (2) and Mn (3)), [Mn{sub 2}(cfH)(odpa)(H{sub 2}O){sub 3}]{center_dot}0.5H{sub 2}O (4), [Co{sub 2}(norfH)(bpta)({mu}{sub 2}-H{sub 2}O)(H{sub 2}O){sub 2}]{center_dot}H{sub 2}O (5) and [Co{sub 3}(saraH){sub 2}(Hbpta){sub 2}(H{sub 2}O){sub 4}]{center_dot}9H{sub 2}O (6) (cfH=ciprofloxacin, norfH=norfloxacin, saraH=sarafloxacin, bpdc=4,4 Prime -biphenyldicarboxylate, odpa=4,4 Prime -oxydiphthalate, bpta=3,3 Prime ,4,4 Prime -biphenyltetracarboxylate) have been synthesized and characterized. Compounds 1-3 consist of 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Compounds 4 and 5 display 2D structures based on tetranuclear manganese or cobalt clusters with (3,6)-connected kgd topology. Compound 6 exhibits a 2D bilayer structure, which represents the first example of metal-quinolone complexes with 2D bilayer structure. By inspection of the structures of 1-6, it is believed that the long aromatic polycarboxylate ligands are important for the formation of 2D metal-quinolone complexes. The magnetic properties of compounds 3-6 was studied, indicating the existence of antiferromagnetic interactions. Furthermore, the luminescent properties of compounds 1-2 are discussed. - Graphical abstract: Six novel 2D metal-quinolone complexes have been prepared by self-assemblies of the quinolones and metal salts in the presence of long aromatic polycarboxylates. Highlights: Black-Right-Pointing-Pointer Compounds 1-3 consist of novel 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Black-Right-Pointing-Pointer Compounds 4 and 5 are two novel 2D layers based on tetranuclear Mn or Co clusters with kgd topology. Black-Right-Pointing-Pointer Compound 6 is the first example of metal-quinolone complexes with 2D bilayer structure. Black-Right-Pointing-Pointer Compounds 1-6 represent six unusual

Solid-state syntheses and single-crystal characterizations of three tetravalent thorium and uranium silicates

International Nuclear Information System (INIS)

Jin, Geng Bang; Soderholm, L.

2015-01-01

Colorless crystals of ThSiO 4 (huttonite) (1) and (Ca 0.5 Na 0.5 ) 2 NaThSi 8 O 20 (2) have been synthesized by the solid-state reactions of ThO 2 , CaSiO 3 , and Na 2 WO 4 at 1073 K. Green crystals of (Ca 0.5 Na 0.5 ) 2 NaUSi 8 O 20 (3) have been synthesized by the solid-state reactions of UO 2 , CaSiO 3 , and Na 2 WO 4 at 1003 K. All three compounds have been characterized by single-crystal X-ray diffraction. Compound 1 adopts a monazite-type three-dimensional condensed structure, which is built from edge- and corner-shared ThO 9 polyhedra and SiO 4 tetrahedra. Compounds 2 and 3 are isostructural and they crystallize in a steacyite-type structure. The structure consists of discrete pseudocubic [Si 8 O 20 ] 8− polyanions, which are connected by An 4+ cations into a three-dimensional framework. Each An atom coordinates to eight monodentate [Si 8 O 20 ] 8− moieties in a square antiprismatic geometry. Na + and Ca 2+ ions reside in the void within the framework. Raman spectra of 1, 2, and 3 were collected on single crystal samples. 1 displays more complex vibrational bands than thorite. Raman spectra of 2 and 3 are analogous with most of vibrational bands located at almost the same regions. - Graphical abstract: A Raman spectrum and crystal structures of (Ca 0.5 Na 0.5 ) 2 NaAnSi 8 O 20 (An=Th, U), which contain pseudocubic [Si 8 O 20 ] 8− polyanions and eight-coordinate An 4+ cations. - Highlights: • Single crystal growth of three tetravalent actinide silicates from melts. • Single-crystal structures and Raman spectra of (Ca 0.5 Na 0.5 ) 2 NaAnSi 8 O 20 (An=Th, U). • First report of Raman spectrum of huttonite on single crystal samples

Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

Energy Technology Data Exchange (ETDEWEB)

Nascimento, A.L.C.S. do; Caires, F.J., E-mail: caires.flavio@yahoo.com.br; Gomes, D.J.C.; Gigante, A.C.; Ionashiro, M.

2014-01-10

Graphical abstract: - Highlights: • The transition metal ion nicotinates were synthesized. • The TG–DTA curves provided previously unreported information about thermal behaviour. • The gaseous products released were detected by TG–DSC coupled to FTIR. - Abstract: Solid-state M(L){sub 2}·nH{sub 2}O compounds, where M stands for bivalent transition metals (Mn, Fe, Co, Ni, Cu and Zn), L is nicotinate and n = 0–4.5, have been synthesized. Characterization and thermal behaviour of these compounds were investigated employing elemental analysis based on the mass losses observed in the TG–DTA curves, complexometry, X-ray diffractometry, infrared spectroscopy (FTIR), simultaneous thermogravimetric and differential thermal analysis (TG–DTA) and TG–DSC coupled to FTIR. The thermal behaviour of nicotinic acid and its sodium salt was also investigated. For the hydrated transition metal compounds, the dehydration and thermal decomposition of the anhydrous compounds occur in a single step. For the sodium nicotinate, the final residue up to 765 °C is sodium carbonate and for the transition metal nicotinates, the final residues are Mn{sub 3}O{sub 4}, Fe{sub 2}O{sub 3}, Co{sub 3}O{sub 4}, NiO, CuO and ZnO. The results also provided information concerning the thermal stability, thermal decomposition and identification of the gaseous products evolved during the thermal decomposition of the compounds.

Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

International Nuclear Information System (INIS)

Nascimento, A.L.C.S. do; Caires, F.J.; Gomes, D.J.C.; Gigante, A.C.; Ionashiro, M.

2014-01-01

Graphical abstract: - Highlights: • The transition metal ion nicotinates were synthesized. • The TG–DTA curves provided previously unreported information about thermal behaviour. • The gaseous products released were detected by TG–DSC coupled to FTIR. - Abstract: Solid-state M(L) 2 ·nH 2 O compounds, where M stands for bivalent transition metals (Mn, Fe, Co, Ni, Cu and Zn), L is nicotinate and n = 0–4.5, have been synthesized. Characterization and thermal behaviour of these compounds were investigated employing elemental analysis based on the mass losses observed in the TG–DTA curves, complexometry, X-ray diffractometry, infrared spectroscopy (FTIR), simultaneous thermogravimetric and differential thermal analysis (TG–DTA) and TG–DSC coupled to FTIR. The thermal behaviour of nicotinic acid and its sodium salt was also investigated. For the hydrated transition metal compounds, the dehydration and thermal decomposition of the anhydrous compounds occur in a single step. For the sodium nicotinate, the final residue up to 765 °C is sodium carbonate and for the transition metal nicotinates, the final residues are Mn 3 O 4 , Fe 2 O 3 , Co 3 O 4 , NiO, CuO and ZnO. The results also provided information concerning the thermal stability, thermal decomposition and identification of the gaseous products evolved during the thermal decomposition of the compounds

Amino acid linked bromobenzoyl thiourea derivatives: syntheses, characterization and antimicrobial activities

International Nuclear Information System (INIS)

Raheel, A.; Din, I.U.; Badshah, A.; Rauf, M.K.; Andleeb, S.

2016-01-01

Five new bromobenzoyl thiourea derivatives (1-5) linked with different amino acids were synthesized via the reaction of bromobenzoyl chloride with potassium thiocyanide and the corresponding amines. The synthetic compounds were characterized by single crystal XRD, IR and NMR (/sup 1/H- and /sup 13/C-) spectroscopy in addition to elemental analysis and melting point determinations. These compounds were also preliminary analyzed for antifungal and antibacterial activity against different strains of fungi and bacteria, respectively. The data suggest that the compounds exhibited promising antimicrobial activity and may prove potential lead compounds as antimicrobial agent. (author)

Nanoscale grain growth behaviour of CoAl intermetallic synthesized ...

Indian Academy of Sciences (India)

Grain growth behaviour of the nanocrystalline CoAl intermetallic compound synthesized by mechanical alloying has been studied by isothermal annealing at different temperatures and durations. X-ray diffraction method was employed to investigate structural evolutions during mechanical alloying and annealing processes.

Nanoscale grain growth behaviour of CoAl intermetallic synthesized ...

Indian Academy of Sciences (India)

Administrator

Abstract. Grain growth behaviour of the nanocrystalline CoAl intermetallic compound synthesized by mechanical alloying has been studied by isothermal annealing at different temperatures and durations. X-ray diffraction method was employed to investigate structural evolutions during mechanical alloying and anneal-.

Synthesis and biological evaluation of schiff bases of 4-aminophenazone as an anti-inflammatory, analgesic and antipyretic agent

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Shahzad Murtaza

2017-01-01

Full Text Available A series of schiff base derivatives of 4-aminophenazone (4APZ-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one with different aldehydes were synthesized. The synthetic compounds were screened for their anti-inflammatory, analgesic and antipyretic activities. The characterization of synthesized compounds was carried out by 1H NMR, 13C NMR and MS. Carrageenan-induced paw oedema (CIPO and histamine induced paw oedema (HIPO methods were used to determine the anti-inflammatory activity of commercial sample of 4APZ and its synthesized schiff bases in mice. The anti-inflammatory activity was in the order of 4APZAB > 4APZBB > 4APZCB > 4APZVn and all the test compounds exhibited considerable dose dependent inhibition of the paw oedema. The effect of the compounds on membrane stabilization was also determined which showed that compounds 4APZ (120 and 240 mg/kg doses, 4APZAB (160 mg/kg and 4APZVn (600 mg/kg produced highly significant inhibition (P  4APZBB > 4APZVn > 4APZCB. Moreover, phenobarbitone-induced sleeping time (PIST in mice was also studied but only 600 mg/kg of 4APZVn significantly increased the duration of induced sleep which also suggested its sedative property. Brewer’s yeast was used to induce fever in rabbits and analysed the compounds for their antipyretic activity. Different doses of 4APZ for different time durations (240 mg/kg-after 1 h, 120 and 240 mg/kg doses-after 2 h produced highly significant (P < 0.001 inhibition of hyperpyrexia. Other compounds showed good antipyretic activity after 2, 3 and 4 h.

Microstructure and Thermal Properties of Polypropylene/Clay Nanocomposites with TiCl4/MgCl2/Clay Compound Catalyst

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Limei Wang

2015-01-01

Full Text Available Polypropylene (PP/clay nanocomposites were synthesized by in situ intercalative polymerization with TiCl4/MgCl2/clay compound catalyst. Microstructure and thermal properties of PP/clay nanocomposites were studied in detail. Fourier transform infrared (FTIR spectra indicated that PP/clay nanocomposites were successfully prepared. Both wide-angle X-ray diffraction (XRD and transmission electron microscopy (TEM examination proved that clay layers are homogeneously distributed in PP matrix. XRD patterns also showed that the α phase was the dominate crystal phase of PP in the nanocomposites. Thermogravimetric analysis (TGA examinations confirmed that thermal stability of PP/clay nanocomposites was markedly superior to pure PP. Differential scanning calorimetry (DSC scans showed that the melt temperature and the crystallinity of nanocomposites were slightly lower than those of pure PP due to crystals imperfections.

Two-dimensional inorganic–organic hybrid semiconductors composed of double-layered ZnS and monoamines with aromatic and heterocyclic aliphatic rings: Syntheses, structures, and properties

Energy Technology Data Exchange (ETDEWEB)

Wang, Sujing; Li, Jing, E-mail: jingli@rutgers.edu

2015-04-15

As an addition to the II–VI based inorganic–organic hybrid semiconductor family, five new two-dimensional (2D) double-layered structures have been synthesized employing monoamines with different aromatic or heterocyclic aliphatic rings. Zn{sub 2}S{sub 2}(bza) (1), Zn{sub 2}S{sub 2}(mbza) (2), Zn{sub 2}S{sub 2}(fbza) (3), Zn{sub 2}S{sub 2}(pca) (4), and Zn{sub 2}S{sub 2}(thfa) (5) (bza=benzylamine, mbza=4-methoxybenzylamine, fbza=4-flurobenzylamine, pca=3-picolylamine, and thfa=tetrahydrofurfurylamine) are prepared by solvothermal reactions and characterized by different analytical methods, including powder X-ray diffraction, optical diffuse reflection, thermogravimetric analysis and photoluminescence spectroscopy. The powder X-ray diffraction patterns show that all five compounds adopt 2D double-layered structures. Optical diffuse reflectance spectra of these compounds suggest that they have notably lower band gaps than those of the similar compounds composed of aliphatic alkyl amines. Their photoluminescence properties and thermal stability are also analyzed. - Graphical abstract: Five new members of two-dimensional double-layered 2D-Zn{sub 2}S{sub 2}(L) (L=Ligand) structures employing monoamines with different aromatic or heterocyclic aliphatic rings have been designed, synthesized, and characterized. - Highlights: • A new sub-family of II-VI based hybrid semiconductors are designed, synthesized, and structurally characterized using amines with aromatic or aliphatic cyclic rings. • These compounds have notably lower band gaps than those made of aliphatic alkyl amines, greatly broadening the range of band gaps of this material family. • They emit strongly with systematically tunable emission intensity and energy.

A facile synthesis and the antimicrobial activity of some 4-aryltriazoles

Directory of Open Access Journals (Sweden)

SHIPRA BALUJA, SUMITRA CHANDA*, RAJESH CHABHADIYA*, NIKUNJ KACHHADIA, RATHISH NAIR* and ASIF SOLANKI

2007-06-01

Full Text Available Some 4-aryltriazoles were synthesized and tested for their antibacterial effects against Bacillus cereus, Pseudomonas testosteroni, Klebsiella pneumoniae Micrococcus flavus, and Citrobacter freundii. The 4-aryltriazoles were obtained by cyclization of the potassium salt of the appropriately substituted dithiocarbazinic acid with aromatic amines. The new synthesized compounds were characterized using infrared and 1H nuclear magnetic resonance spectroscopy and further supported by mass spectrometry.

Synthesis and antitumor evaluation of some new N4 substituted sulfa pyridine derivatives with studying the synergistic effect of γ-irradiation

International Nuclear Information System (INIS)

Elsaid Agha, H.M.S.

2011-01-01

The aim of the present investigation is to synthesize a new class of N 4 substituted sulfa pyridine derivatives with anticipated cytotoxic activity. All the newly synthesized compounds were screened for their in-vitro cytotoxic activity against breast cancer cell line (MCF-7) compared to the reference drug Doxorubicin. Also the synergism of the most potent synthesized compounds with γ- radiation was studied. Moreover, a molecular docking study was carried out by docking the most active synthesized compounds in the active site of Cyclin Dependent Kinase 2 receptor to assess their inhibitory effect upon this enzyme as this may have a role in their anticancer activity.

Discovery of 2-(4-Substituted-piperidin/piperazine-1-yl-N-(5-cyclopropyl-1H-pyrazol-3-yl-quinazoline-2,4-diamines as PAK4 Inhibitors with Potent A549 Cell Proliferation, Migration, and Invasion Inhibition Activity

Directory of Open Access Journals (Sweden)

Tianxiao Wu

2018-02-01

Full Text Available A series of novel 2,4-diaminoquinazoline derivatives were designed, synthesized, and evaluated as p21-activated kinase 4 (PAK4 inhibitors. All compounds showed significant inhibitory activity against PAK4 (half-maximal inhibitory concentration IC50 < 1 μM. Among them, compounds 8d and 9c demonstrated the most potent inhibitory activity against PAK4 (IC50 = 0.060 μM and 0.068 μM, respectively. Furthermore, we observed that compounds 8d and 9c displayed potent antiproliferative activity against the A549 cell line and inhibited cell cycle distribution, migration, and invasion of this cell line. In addition, molecular docking analysis was performed to predict the possible binding mode of compound 8d. This series of compounds has the potential for further development as PAK4 inhibitors for anticancer activity.

Thermoluminescence properties of Li2B4O7:Cu, B phosphor synthesized using solution combustion technique

Science.gov (United States)

Ozdemir, A.; Altunal, V.; Kurt, K.; Depci, T.; Yu, Y.; Lawrence, Y.; Nur, N.; Guckan, V.; Yegingil, Z.

2017-12-01

To determine the effects of various concentrations of the activators copper (Cu) and boron (B) on the thermoluminescence (TL) properties of lithium tetraborate, the phosphor was first synthesized and doped with five different concentrations of copper (0.1-0.005 wt%) using solution combustion method. 0.01 wt% Cu was the concentration which showed the most significant increase in the sensitivity of the phosphor. The second sort of Li2B4O7:Cu material was prepared by adding B (0.001-0.03 wt%) to it. The newly developed copper-boron activated lithium tetraborate (Li2B4O7:Cu, B) material with 0.01 wt% Cu and 0.001 wt% B impurity concentrations was shown to have promise as a TL phosphor. The material formation was examined using powder x-Ray Diffraction (XRD) analysis and Scanning Electron Microscope (SEM) imaging. Fourier Transform Infrared (FT-IR) spectrum of the synthesized polycrystalline powder sample was also recorded. The TL glow curves were analyzed to determine various dosimetric characteristics of the synthesized luminophosphors. The dose response increased in a ;linear; way with the beta-ray exposure between 0.1-20 Gy, a dose range being interested in medical dosimetry. The response with changing photon and electron energy was studied. The rate of decay of the TL signal was investigated both for dark storage and under direct sunlight. Li2B4O7:Cu, B showed no individual variation of response in 9 recycling measurements. The fluorescence spectrum was determined. The kinetic parameters were estimated by different methods and the results discussed. The studied properties of synthesized Li2B4O7:Cu, B were found all favorable for dosimetric purposes.

Design and Syntheses of Novel Fluoroporphyrin-Anthraquinone Complexes as Antitumor Agents.

Science.gov (United States)

Yang, Gu-Liang; Zhao, Sheng-Fang; Chen, Nian-You; Li, Shiming

2016-01-01

A novel fluoroporphyrin-anthraquinone hybrid with dipeptide link and its metal complexes were synthesized and evaluated for anti-proliferation activity in human cancer cell line HeLa. The preliminary results demonstrated that all the compounds showed moderate to excellent antitumor activities. Among the active compounds, compound 3 which contains fluorinated porphyrin-anthraquinone and zinc ion exhibited the highest potency with IC50 value of 8.83 µM, indicating that it was a promising antitumor candidate.

Synthesis of 3-(4, 5-dihydro-1-phenyl-5-substituted phenyl-1H-pyrazol-3-yl-2H-chromen-2-one derivatives and evaluation of their anticancer activity

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Nitin Kumar

2017-05-01

Full Text Available A novel series of 3-(4, 5-dihydro-1-phenyl-5-substituted phenyl-1H-pyrazol-3-yl-2H-chromen-2-one derivatives were synthesized. In the first step salicylaldehyde was reacted with ethylacetoacetate at room temperature by stirring which gives compound (I. Compound (I when refluxed with substituted benzaldehyde and diethylamine in the presence of n-butanol for 4–5 h gives substituted derivatives (IIa–d. Compounds synthesized in step 2 when refluxed with phenyl hydrazine in the presence of pyridine for 6–7 h gives the title compounds (IIIa–d. All the synthesized compounds were sent to NCI for anticancer activity. Synthesized compounds were tested for anticancer activity against 60 different cell lines. From the data thus obtained it was observed that simple coumarin ring derivatives were more effective in inhibiting the growth of cancerous cell lines, than coumarin-pyrazoline derivatives. Among all the synthesized compounds, irrespective of compounds having simple coumarin ring and coumarin-pyrazoline combination, compounds IIa–c, IIIb and IIId were potent anticancer agents. Compounds were active for the single dose therapeutic program at the dose of 1.00E-5 molar concentration. The main anti cancer activity is assumed to be due to the presence of the lactone structure in coumarin moiety.

Fabrication and characterization of nanostructured Fe3S4, an isostructural compound of half-metallic Fe3O4

KAUST Repository

Li, Peng; Xia, Chuan; Zhang, Qiang; Guo, Zaibing; Cui, Wenyao; Bai, Haili; Alshareef, Husam N.; Zhang, Xixiang

2015-01-01

High-purity, well-crystallized spinel Fe3S4 nanoplatelets were synthesized by the hydrothermal method, and the saturation magnetic moment of Fe3S4 was measured at 1.83 μB/f.u. The temperature-dependent resistivity of Fe3S4 was metallic

Synthesis and electrochemical properties of Li4Ti5O12

CSIR Research Space (South Africa)

Liu, GQ

2011-06-01

Full Text Available The spinel compound Li4Ti5O12 was synthesized by a solid state method. In this synthesizing process, anatase TiO2 and Li2CO3 were used as reactants. The influences of reaction temperature and calcination time on the properties of products were...

Synthesis and crystal structure of hydrogen selenates K(HSeO4)(H2SeO4) and Cs(HSeO4)(H2SeO4)

International Nuclear Information System (INIS)

Troyanov, S.I.; Morozov, I.V.; Zakharov, M.A.; Kemnitz, E.

1999-01-01

Hydrogen selenates of the compositions K(HSeO 4 )(H 2 SeO 4 ) and Cs(HSeO 4 )(H 2 SeO 4 ) are synthesized by the reaction of alkali metal carbonates with an excess of the concentrated selenic acid. The X-ray diffraction study showed that both compounds are isostructural to the corresponding hydrogen sulfates. The difference in the systems of hydrogen bonding are caused by various combinations of the acceptor functions of the oxygen atoms in the HSeO 4 and H 2 SeO 4 groups

Thermoluminescence properties of Li2B4O7:Cu, B phosphor synthesized using solution combustion technique

International Nuclear Information System (INIS)

Ozdemir, A.; Altunal, V.; Kurt, K.; Depci, T.; Yu, Y.; Lawrence, Y.; Nur, N.; Guckan, V.; Yegingil, Z.

2017-01-01

To determine the effects of various concentrations of the activators copper (Cu) and boron (B) on the thermoluminescence (TL) properties of lithium tetraborate, the phosphor was first synthesized and doped with five different concentrations of copper (0.1–0.005 wt%) using solution combustion method. 0.01 wt% Cu was the concentration which showed the most significant increase in the sensitivity of the phosphor. The second sort of Li 2 B 4 O 7 :Cu material was prepared by adding B (0.001–0.03 wt%) to it. The newly developed copper-boron activated lithium tetraborate (Li 2 B 4 O 7 :Cu, B) material with 0.01 wt% Cu and 0.001 wt% B impurity concentrations was shown to have promise as a TL phosphor. The material formation was examined using powder x-Ray Diffraction (XRD) analysis and Scanning Electron Microscope (SEM) imaging. Fourier Transform Infrared (FT-IR) spectrum of the synthesized polycrystalline powder sample was also recorded. The TL glow curves were analyzed to determine various dosimetric characteristics of the synthesized luminophosphors. The dose response increased in a “linear” way with the beta-ray exposure between 0.1–20 Gy, a dose range being interested in medical dosimetry. The response with changing photon and electron energy was studied. The rate of decay of the TL signal was investigated both for dark storage and under direct sunlight. Li 2 B 4 O 7 :Cu, B showed no individual variation of response in 9 recycling measurements. The fluorescence spectrum was determined. The kinetic parameters were estimated by different methods and the results discussed. The studied properties of synthesized Li 2 B 4 O 7 :Cu, B were found all favorable for dosimetric purposes. - Highlights: • Li 2 B 4 O 7 :Cu, B synthesis using solution combustion method with various concentrations. • Structure analysis of Li 2 B 4 O 7 :Cu, B using XRD, SEM and FTIR methods. • Investigation of thermoluminescent properties of Li 2 B 4 O 7 :Cu, B. • Relatively good

Synthesis of novel pyrazolo[3,4-d]pyrimidinone derivatives as cytotoxic inhibitors

Directory of Open Access Journals (Sweden)

Ameur Rahmouni

2014-02-01

Full Text Available Various α-fonctionalized iminoethers 2 were easily prepared from ethyl 5-amino-3-substituted-1-phenyl-1H-pyrazole-4-carboxylate 1. The reaction of iminoethers 2 with ammonia afforded 3-substitued-1-phenyl-1H-pyrazolo[3,4-d] pyrimidin-4(5H-ones 3 which were also synthesized by the addition of formamide to ethyl 5-amino-3-substituted-1-phenyl-1H-pyrazole-4-carboxylate 1. The 5-amino-3-substitued-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H-ones 4 were obtained from hydrazonolysis of iminoethers 2. Otherwise, the condensation of these intermediates 2 with a series of some primary amines and hydroxylamine led respectively, to the corresponding 3,5-disubstitued-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H-ones 5 and the 3-substitued-5-hydroxy-1-phenyl-1H-pyrazolo[3,4-d] pyrimidin-4-(5H-ones 6. The synthesized compounds 1-6 were completely characterized by 1H NMR, 13C NMR, IR and HRMS. Some synthesized compounds were evaluated for their cytotoxic effect using the Human cervical adenocarcinoma Hela cell line.

5-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione

Directory of Open Access Journals (Sweden)

Salman A. Khan

2010-03-01

Full Text Available The title compound, 5-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione, has been synthesized by condensation of 1,3-diethyl-2-thiobarbituric acid and 3,5-dimethyl-1-phenylpyrazole-4-carbaldehyde in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and EI-MS spectral analysis.

Synthesis and Antifungal Activities of 5-(o-Hydroxy phenyl-2-[4'aryl-3'chloro-2'azetidinon-1-yl]-1,3,4-thiadiazole

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Shiv K. Gupta

2011-01-01

Full Text Available New series of 5-(o-hydroxy phenyl-2-[4'aryl-3'chloro-2'azetidinon-1-yl]-1,3,4-thiadiazole have been synthesized and the structures of the new compounds were established on the basis of IR, 1H NMR spectral data. In vitro antifungal activity (MIC activity was evaluated and compared with standard drugs of ketoconazole. Compounds 3c in the series has shown interesting antifungal activity against both C. albicans and A. niger fungus. In the gratifying result, most of the compounds were found to have moderate antifungal activity.

3,4-Dimethoxybenzohydrazide derivatives as antiulcer: Molecular modeling and density functional studies.

Science.gov (United States)

Taha, Muhammad; Ismail, Nor Hadiani; Zaki, Hamizah Mohd; Wadood, Abdul; Anouar, El Hassane; Imran, Syahrul; Yamin, Bohari M; Rahim, Fazal; Ali, Muhammad; Khan, Khalid Mohammed

2017-12-01

3,4-Dimethoxybenzohydrazide derivatives (1-25) have been synthesized and evaluated for their urease inhibitory potential. Among the series, compounds 2, 3, 4 and 5 with IC 50 values 12.61 ± 0.07, 18.24 ± 0.14, 19.22 ± 0.21, and 8.40 ± 0.05 µM, respectively, showed excellent urease inhibitory potentials when compared with standard thiourea (IC 50 value 21.40 ± 0.21 µM). Compounds 1, 6, 8, 18, 19 and 20 also showed good to moderate inhibition, while the remaining compounds were found to be completely inactive. The structures of compounds 6 and 25 were confirmed through X-ray crystallography while the structures of remaining compounds were confirmed through ESI-MS and 1 H NMR. Molecular docking studies were performed understand the binding interactions with enzyme active site. The synthesized compounds were evaluated for cytotoxicity and found to be nontoxic. Copyright © 2017 Elsevier Inc. All rights reserved.

Effects of two newly synthesized analogues of lidocaine on rat arterial blood pressure and heart rate.

Science.gov (United States)

Al Rasheed, N M; Al Sayed, M I; Al Zuhair, H H; Al Obaid, A R; Fatani, A J

2001-04-01

Two new analogues of lidocaine were synthesized at the College of Pharmacy, King Saud University: compound I (Methyl-2-[2-(N,N-diethylamino) acetamido]-3-cyano-4,5-dimethylbenzoate) and compound II (Methyl-2-[2-(piperidino) acetamido]-3-cyano-4,5-dimethylbenzoate). Their influence on the arterial blood pressure and the heart rate of urethane-anaesthetized rats was studied and compared with the actions of lidocaine. Compounds I, II and lidocaine induced significant dose-dependent decreases in the arterial blood pressure and heart rate, which usually returned to basal values within 3-5 min. There were significant differences in the potency of the three compounds in producing their effects on blood pressure and heart rate (Plidocaine and compound I, respectively. The results of this study also indicated the ineffectiveness of antagonists of autonomic, histaminergic and 5-HT receptor, and various vasodilators in blocking the actions of the three compounds on blood pressure and heart rate. Pretreatment with CaCl(2)significantly reduced the hypotension and bradycardia induced by the three compounds, suggesting the involvement of calcium channels, probably of the L type. Several possible mechanisms are postulated. In conclusion, the results direct attention to the capability of the two new compounds to decrease blood pressure and heart rate; affects that may have clinical potential. Copyright 2001 Academic Press.

The syntheses of radiolabelled Org 5222 and its main metabolite Org 30526

International Nuclear Information System (INIS)

Vader, Jan; Kaspersen, Frans; Sperling, Eric; Schlachter, Irene; Terpstra, Annie; Hilberink, Peter; Wagenaars, Gerard

1994-01-01

The syntheses of trans-5-chloro-2,3,3a-12b-tetrahydro-2-methyl-1H-dibenz[2,3:6,7] oxepino[4 ,5-c]pyrrole (Org 5222), a potential antipsychotic compound, labelled with 3 H, 14 C and 36 Cl and trans-5-chloro-2,3,3a,12b-tetrahydro-1H-dibenz[2,3:6,7]-oxepino[4, 5-c] pyrrole (Org 30526) labelled with 3 H are described. 3 H-labelled Org 5222 of low specific activity was prepared by a base catalyzed exchange with tritiated water of an amide precursor, 3 H-labelled Org 5222 with a high specific activity by a catalytic reductive dehalogenation. 3 H-labelled Org 30526 was prepared both by demethylation of 3 H-Org 5222 and by catalytic reductive iodination of 11-iodo-Org 30526. 14 C-labelled Org 5222 was synthesized in 6 steps using 14 C-sarcosine as starting material. 36 Cl-labelled Org 5222 was prepared by diazotation reaction in the presence of H 36 Cl. (author)

Different properties of polysialic acids synthesized by the polysialyltransferases ST8SIA2 and ST8SIA4.

Science.gov (United States)

Mori, Airi; Hane, Masaya; Niimi, Yuki; Kitajima, Ken; Sato, Chihiro

2017-09-01

Polysialic acid (polySia) is mainly found as a modification of neural cell adhesion molecule (NCAM) in whole embryonic brains, as well as restricted areas of adult vertebrate brains, including the hippocampus. PolySia shows not only repulsive effects on NCAM-involved cell-cell interactions due to its bulky and hydrated properties, but also attractive effects on the interaction with neurologically active molecules, which exerts a reservoir function. Two different polysialyltransferases, ST8SIA2 and ST8SIA4, are involved in the synthesis of polySia chains; however, to date, the differences of the properties between polySia chains synthesized by these two enzymes remain unknown. In this study, to clarify this point, we first prepared polySia-NCAMs from HEK293 cells stably expressing ST8SIA4 and ST8SIA2, or ST8SIA2 (SNP-7), a mutant ST8SIA2 derived from a schizophrenia patient. The conventional sensitive chemical and immunological characterizations showed that the quantity and quality (structural features) of polySia are not so much different between ST8SIA4- and ST8SIA2-synthesized ones, apart from those of ST8SIA2 (SNP-7). Then, we assessed the homophilic and heterophilic interactions mediated by polySia-NCAM by adopting a surface plasmon resonance measurement as an in vitro analytical method. Our novel findings are as follows: (i) the ST8SIA2- and ST8SIA4-synthesized polySia-NCAMs exhibited different attractive and repulsive effects than each other; (ii) both polySia- and oligoSia-NCAMs synthesized by ST8SIA2 were able to bind polySia-NCAMs; (iii) the polySia-NCAM synthesized by a ST8SIA2 (SNP-7) showed markedly altered attractive and repulsive properties. Collectively, polySia-NCAM is suggested to simultaneously possess both attractive and repulsive properties that are highly regulated by the two polysialyltransferases. © The Author 2017. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Electronic structure and magnetic properties of FeWO{sub 4} nanocrystals synthesized by the microwave-hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Almeida, M.A.P. [INCTMN-DQ-Universidade Federal de Sao Carlos, Sao Carlos, P.O. Box 676, 13565-905, SP (Brazil); Cavalcante, L.S., E-mail: laeciosc@bol.com.br [INCTMN-Universidade Estadual, Paulista, P.O. Box 355, 14801-907, Araraquara, SP (Brazil); Morilla-Santos, C.; Filho, P.N. Lisboa [MAv-Universidade Estadual, Paulista, P.O. Box 473, 17033-360, Bauru, SP (Brazil); Beltran, A.; Andres, J.; Gracia, L. [Department de Quimica Fisica i Analitica, Universitat Jaume I, E-12071 Castello (Spain); Longo, E. [INCTMN-DQ-Universidade Federal de Sao Carlos, Sao Carlos, P.O. Box 676, 13565-905, SP (Brazil); INCTMN-Universidade Estadual, Paulista, P.O. Box 355, 14801-907, Araraquara, SP (Brazil)

2012-11-15

This communication reports that FeWO{sub 4} nanocrystals were successfully synthesized by the microwave-hydrothermal method at 443 K for 1 h. The structure and shape of these nanocrystals were characterized by X-ray diffraction, Rietveld refinement, and transmission electron microscopy. The experimental results and first principles calculations were combined to explain the electronic structure and magnetic properties. Experimental data were obtained by magnetization measurements for different applied magnetic fields. Theoretical calculations revealed that magnetic properties of FeWO{sub 4} nanocrystals can be assigned to two magnetic orderings with parallel or antiparallel spins in adjacent chains. These factors are crucial to understanding of competition between ferro- and antiferromagnetic behavior. Highlights: Black-Right-Pointing-Pointer Monophasic FeWO{sub 4} nanocrystals were synthesized by the microwave-hydrothermal method. Black-Right-Pointing-Pointer Rietveld refinement and clusters model for monoclinic structure Black-Right-Pointing-Pointer Magnetic properties of FeWO{sub 4} nanocrystals at different temperatures.

Synthesis and electrochemical properties of LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12

CSIR Research Space (South Africa)

Liu, GQ

2011-08-01

Full Text Available Spinel compound LiNi0.4Mn1.5Cr0.1O4 (LNMCO) and Li4Ti5O12 (LTO) were synthesized by the sol-gel method and the solid-state method, respectively. The particle sizes of the products LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12 were 0.5 to 2 um and 0.5 to 0.8 um...

Supercapacitors studies on BiPO4 nanoparticles synthesized via a simple microwave approach

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S. Vadivel

2017-07-01

Full Text Available BiPO4 nanomaterial was synthesized using EDTA (ethylene diamine tetra acetic acid as the surfactant via a simple microwave method. The structure and morphology of BiPO4 were systematically characterized by X-ray diffraction (XRD, Fourier-transform infrared spectroscopy (FT-IR, and scanning electron microscopy (FE-SEM studies. The obtained BiPO4 nanoparticles were, on average, 150–300 nm. The electrochemical results showed that the specific capacitance of BiPO4 obtained using the microwave route was up to 104 Fg−1 at a current density of 1 Ag−1 with a large potential window of 1.7 V. The material showed excellent cycling stability (92% capacitance retention after 500 cycles at a current density of 1 Ag−1.

6-Bromo-2-(1,4-dibromo-4-methylcyclohexyl-6-methylheptan-4-one

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Ahmed Benharref

2017-11-01

Full Text Available The title compound, C15H25Br3O, was synthesized in one step from a mixture of α-atlantone [2-methyl-6-(4-methylcyclohex-3-en-1-ylhepta-2,5-dien-4-one] and γ-atlantone [2-methyl-6-(4-methylcyclohex-3-en-1-ylidenehept-2-en-4-one], which were isolated from an essential oil of the Atlas cedar (Cedrus Atlantica. The molecule is built up from the bromo ethyl cyclohexane ring, which has a substituent bromomethylhexanone group. The cyclohexane ring adopts a chair conformation. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming zigzag chains parallel to [100].

Synthesis of novel 4H-1,2,4-triazole-3-thiol derivatives with 2-(2,6-dichlorophenylaminobenzyl fragment in molecules and their anti-inflammatory activity

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Yu. L. Shepeta

2016-04-01

Full Text Available Aim. The study of anti-inflammatory activity of novel 4H-1,2,4-triazole-3-thiol derivatives is one of the most priority direction of pharmacological investigation of mentioned heterocyclic system. Methods and results. Based on the heterocyclization reaction of N-substituted thiosemicarbazides in alkaline medium the synthesis of novel non-condensed derivatives with 4H-1,2,4-triazole and 2-(2,6-dichlorophenylaminobenzyl fragments was carried out. Further chemical modification of synthesized 5-[2-(2,6-dichlorophenylaminobenzyl]-4H-1,2,4-triazole-3-thioles was performed via S-alkylation reactions with N-aryl(thiophene-2-ylsubstituted 2-chloroacetamides and 2-chloro-1-(3,5-diaryl-4,5-dihydropyrazol-1-ylethanones. Structure of synthesized compounds was confirmed by the elemental analysis and 1H NMR spectral data. Conclusions. The research of anti-inflammatory activity has been conducted on the carrageenan-induced edema of the rat’s extremities model. The results allow to identify highly active compounds 2-{5-[2-(2,6-dichloro-phenylamino-benzyl]-4-ethyl-4Н-[1,2,4]triazol-3-ylsulfanyl}-N-(4-chlorophenylacetamide (compound 3b and 2-{5-[2-(2,6-dichloro-phenylamino-benzyl]-4-ethyl-4Н-[1,2,4]triazol-3-ylsulfanyl}-1-[5-(4-methoxy-phenyl-3-(naphthalen-2-yl-4,5-dihydro-pyrazol-1-yl]-ethanone (compound 5c with evident antiexudative effect comparable with the same effect of diclofenac sodium.

Organic compounds generated after the flow of water through micro-orifices: Were they synthesized?

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Tomiichi Hasegawa

2017-08-01

organic compounds are synthesized from nonorganic matter in air or CO2 dissolved in water by the action of hydroxyl radicals generated by flows through micro-orifices.

One-pot synthesis of carbazole based 3-hydroxy-4H-chromen-4-ones by modified Algar-Flynn-Oyamada reaction and their antimicrobial activity

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Ashok Dongamanti

2015-01-01

Full Text Available A new series of 2-(9-ethyl-9H-carbazol-3-yl-3-hydroxy-4Hchromen-4-ones have been synthesized from substituted 2-hydroxy acetophenones and 9-ethyl-9H-carbazole-3-carbaldehyde using NaOH and H2O2 by modified Algar-Flynn-Oyamada reaction. In this method flavonols are synthesized without isolating chalcones in good yields (70-82%. The structures of the compounds were established on the basis of 1H-NMR, 13CNMR, FT-IR and mass spectral and analytical data. All the compounds were evaluated for their antimicrobial activity against bacteria such as Staphylococus aureus, Bacillus subtilis, Escherichia coli and Klebsiella pneumoniae as well as fungi such as Aspergillus flavus and Fusarium oxysporum.

A simplified one-pot synthesis of 9-[(3-[18F]Fluoro-1-hydroxy-2-propoxy)methyl]guanine([18F]FHPG) and 9-(4-[18F]Fluoro-3-hydroxymethylbutyl)guanine ([18F]FHBG) for gene therapy

International Nuclear Information System (INIS)

Shiue, Grace G.; Shiue, Chyng-Yann; Lee, Roland L.; MacDonald, Douglas; Hustinx, Roland; Eck, Stephen L.; Alavi, Abass A.

2001-01-01

9-[(3-[ 18 F]Fluoro-1-hydroxy-2-propoxy)methyl]guanine ([ 18 F]FHPG, 2) has been synthesized by nucleophilic substitution of N 2 -(p-anisyldiphenylmethyl)-9-{[1-(p-anisyldiphenylmethoxy)-3 -toluenesulfonyloxy-2-propoxy]methyl}guanine (1) with potassium [ 18 F]fluoride/Kryptofix 2.2.2 followed by deprotection with 1 N HCl and purification with different methods in variable yields. When both the nucleophilic substitution and deprotection were carried out at 90 deg. C and the product was purified by HPLC (method A), the yield of compound 2 was 5-10% and the synthesis time was 90 min from EOB. However, if both the nucleophilic substitution and deprotection were carried out at 120 deg. C and the product was purified by HPLC, the yield of compound 2 decreased to 2%. When compound 2 was synthesized at 90 deg. C and purified by Silica Sep-Pak (method B), the yield increased to 10-15% and the synthesis time was 60 min from EOB. Similarly, 9-(4-[ 18 F]fluoro-3-hydroxymethylbutyl)guanine ([ 18 F]FHBG, 4) was synthesized with method A and method B in 9% and 10-15% yield, respectively, in a synthesis time of 90 and 60 min, respectively, from EOB. Compound 2 was relatively unstable in acidic medium at 120 deg. C while compound 4 was stable under the same condition. Both compound 2 and compound 4 had low lipid/water partition coefficient (0.126±0.022, n=5 and 0.165±0.023, n=5, respectively). Although it contains non-radioactive ganciclovir (∼5-30 μg) as a chemical by-product, compound 2 synthesized by method B has a similar uptake in 9L glioma cells as that synthesized by method A, and is a potential tracer for imaging herpes simplex virus thymidine kinase gene expression in tumors using PET. Similarly, compound 4 synthesized by method B contains ∼10-25 μg of penciclovir as a chemical by-product. Thus, the simplified one pot synthesis (method B) is a useful method for synthesizing both compound 2 and compound 4 in good yield for routine clinical use, and the method is

ANTIMICROBIAL ACTIVITY OF [1,2,4]TRIAZOLO[4,3-а]PYRAZIN-8(7H-ONE DERIVATIVES

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Kulikovska K. Yu.

2014-12-01

Full Text Available Today the problem of microbial resistance to antibacterial agents becomes the global one. Antimicrobial drugs that are in the pharmaceutical market do not satisfy the needs of modern treatment regimens, particularly Hospitalacquired infections. Therefore, the search for new and effective means of this pharmacological group is an important task of medical chemistry. From the literature it is known that derivatives of [1,2,4]triazolo[4,3-a]pyrazine show a wide range of biological actions, including antimicrobial and fungicidal. This makes it relevant microbiological study of primary derivatives of [1,2,4]triazolo[4,3-a]pyrazine for identifying promising compounds of the series and then study it in biological experiment.Using the PASS C&T (Prediction Activity Spectra for Substances: Complex & Training program and based on published data, we have generated virtual library of derivatives of [1,2,4]triazolo[4,3-a]pyrazine. As a result, we have received 35 new synthetic compounds of 7 series that were not previously described in the literature. Materials and methods The research of antimicrobial and fungicidal activity of the synthesized compounds was carried out in the laboratory of antimicrobial agents GA "Mechnikov Institute of microbiology and immunology" under the leadership of PhD, senior scientist V.V.Kazmirchuka. The activity of the synthesized compounds were studied by conventional method of the two-fold serial dilutions in liquid and solid nutrient medium. For primary screening we have used a set of clinical and reference strains of microorganism: Escherichia coli ATCC 25922 (F-50, Staphylococcus aureus ATCC 25923 (F-49, Bacillus anthracoides ATCC 1312, Pseudomonas aeruginosa ATCC 27853, Candida albicans ATCC 885-653. As the reference preparations were chosen Palin - modern antimicrobial agent of class of fluoroquinolones, Nevigramon - nalidixic acid derivative and Fluconazole -38 Annals of Mechnikov Institute, N 4, 2014 www

Microwave assisted synthesis and antimicrobial activity of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones

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Dongamanti Ashok

2015-06-01

Full Text Available A series of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones were design and synthesized by Click reaction followed by Claisen-Schmidt condensation under microwave irradiation and conventional heating methods. The structures of newly synthesized compounds have been established on the basis of elemental analysis, IR, 1H & 13C NMR and mass spectral data. All the compounds were screened for their antimicrobial activity.

X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

Science.gov (United States)

Varberg, Thomas D.; Skakuj, Kacper

2015-01-01

Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

Preparation, GIAO NMR Calculations and Acidic Properties of Some Novel 4,5-dihydro-1H-1,2,4-triazol-5-one Derivatives with Their Antioxidant Activities

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Havva Aksu

2008-01-01

Full Text Available Six novel 3-alkyl(aryl-4-(p-nitrobenzoylamino-4,5-dihydro-1H-1,2,4-triazol-5- ones (2a-f were synthesized by the reactions of 3-alkyl(aryl-4-amino-4,5-dihydro-1H- 1,2,4-triazol-5-ones (1a-f with p-nitrobenzoyl chloride and characterized by elemental analyses and IR, 1H-NMR, 13C-NMR and UV spectral data. The newly synthesized compounds 2 were titrated potentiometrically with tetrabutylammonium hydroxide in four non-aqueous solvents such as acetone, isopropyl alcohol, tert-butyl alcohol and N,Ndimethylformamide, and the half-neutralization potential values and the corresponding pKa values were determined for all cases. Thus, the effects of solvents and molecular structure upon acidity were investigated. In addition, isotropic 1H and 13C nuclear magnetic shielding constants of compounds 2 were obtained by the gauge-including-atomic-orbital (GIAO method at the B3LYP density functional level. The geometry of each compound has been optimized using the 6-311G basis set. Theoretical values were compared to the experimental data. Furthermore, these new compounds and five recently reported 3-alkyl-4-(2- furoylamino-4,5-dihydro-1H-1,2,4-triazol-5-ones (3a-c,e,f were screened for their antioxidant activities.

Magnetically Recoverable Supported Ruthenium Catalyst for Hydrogenation of Alkynes and Transfer Hydrogenation of Carbonyl Compounds

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A ruthenium (Ru) catalyst supported on magnetic nanoparticles (NiFe2O4) has been successfully synthesized and used for hydrogenation of alkynes at room temperature as well as transfer hydrogenation of a number of carbonyl compounds under microwave irradiation conditions. The cata...

Potential antimicrobial agents from triazole-functionalized 2H-benzo[b][1,4]oxazin-3(4H)-ones.

Science.gov (United States)

Bollu, Rajitha; Banu, Saleha; Bantu, Rajashaker; Reddy, A Gopi; Nagarapu, Lingaiah; Sirisha, K; Kumar, C Ganesh; Gunda, Shravan Kumar; Shaik, Kamal

2017-12-01

A series of substituted triazole functionalized 2H-benzo[b][1,4]oxazin-3(4H)-ones were synthesized by employing click chemistry and further characterized based on 1 H NMR, 13 C NMR, IR and mass spectral studies. All the synthesized derivatives were screened for their in vitro antimicrobial activities. Further, molecular docking studies were accomplished to explore the binding interactions between 1,2,3-triazol-4-yl-2H-benzo[b][1,4]oxazin-3(4H)-one and the active site of Staphylococcus aureus (CrtM) dehydrosqualene synthase (PDB ID: 2ZCS). These docking studies revealed that the synthesized derivatives showed high binding energies and strong H-bond interactions with the dehydrosqualene synthase validating the observed antimicrobial activity data. Based on antimicrobial activity and docking studies, the compounds 9c, 9d and 9e were identified as promising antimicrobial leads. Copyright © 2017 Elsevier Ltd. All rights reserved.

Lanthanide-organic frameworks constructed from multi-functional ligands: Syntheses, structures, near-infrared and visible photoluminescence properties

International Nuclear Information System (INIS)

Li Xinfa; Xie Zailai; Lin Jingxiang; Cao Rong

2009-01-01

A series of multi-functional ligands supported lanthanide-organic frameworks, formulated as [Ln(HL 1 )(H 2 L 2 ) 0.5 (H 4 L 2 ) 0.5 (H 2 O)].(H 2 O) 1.5 .{Ln=La (1), Pr (2), Nd (3), Sm (4), Eu (5); H 3 L 1 =5-Sulfosaclicylic acid; H 4 L 2 =N,N'-piperazine (bis-methylene phosphonic acid)}, have been synthesized by hydrothermal reactions. Single crystal X-ray diffractions and powder XRD patterns confirm they are isostructural. They feature 3D framework structures based on extension of a 'zigzag' inorganic chain by organic linkers. Moreover, the photoluminescence properties of 5 and 3 have been investigated, and they show strong solid-state emissions in the visible and near-infrared (IR) regions at room temperature. - Graphical abstract: Five multi-functional ligands supported 3D lanthanide-organic frameworks have been synthesized and structurally characterized. Compounds 5 and 3 displayed strong solid-state emissions in the visible and near-infrared region at room temperature.

Design and Characterization of a 5.2 GHz/2.4 GHz Fractional- Frequency Synthesizer for Low-Phase Noise Performance

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Dai Foster F

2006-01-01

Full Text Available This paper presents a complete noise analysis of a -based fractional- phase-locked loop (PLL based frequency synthesizer. Rigorous analytical and empirical formulas have been given to model various phase noise sources and spurious components and to predict their impact on the overall synthesizer noise performance. These formulas have been applied to an integrated multiband WLAN frequency synthesizer RFIC to demonstrate noise minimization through judicious choice of loop parameters. Finally, predicted and measured phase jitter showed good agreement. For an LO frequency of 4.3 GHz, predicted and measured phase noise was rms and rms, respectively.

Novel synthesis and antitumor evaluation of polyfunctionally substituted heterocyclic compounds derived from 2-cyano-N-(3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophen-2-yl)-acetamide.

Science.gov (United States)

Shams, Hoda Z; Mohareb, Rafat M; Helal, Maher H; Mahmoud, Amira E

2010-12-27

The reaction of 2-amino-3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophene with ethyl cyanoacetate gave 2-cyano-N-(3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophen-2-yl)-acetamide. The latter was used to synthesize different heterocyclic derivatives comprising thiophene, thiazole, pyrazole, pyridine, pyrimidine, and coumarin rings. The mechanistic and synthetic pathways depended on regioselective attack and/or cyclization by the cyanoacetamido moiety in the key precursor on various chemical reagents. The competition of the reaction pathways including dipolar cyclization, dinucleophilic-bielectrophilic attack, β-attack, Gewald-type attack, and condensation reactions led to the diversity of the synthesized products. The antitumor activities of the synthesized products were studied and evaluated. Most of the compounds revealed high inhibitory effects when screened in vitro for their antiproliferative activity. Three human cancer cell lines, namely, breast adenocarcinoma (MCF-7), non-small cell lung cancer (NCI-H460) and CNS cancer (SF-268) were used in the screening tests. The simplicity of the synthetic procedures which mainly involved one-pot reactions under mild reaction conditions, the convenience of yield production and the diversity of the reactive sites in the produced systems play a valuable role for further heterocyclic transformations and further biological investigations.

Poly[di-μ4-benzene-1,4-dicarboxylato-μ6-succinato-diholmium(III

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Qin He

2008-01-01

Full Text Available The title compound, [Ho2(C4H4O4(C8H4O42]n, was synthesized hydrothermally. The Ho atom is coordinated by four O atoms from four benzene-1,4-dicarboxylate (BDC anions and four O atoms from three succinate anions, in a distorted square-antiprismatic coordination geometry. The antiprisms are bridged by the benzene-1,4-dicarboxylate and succinate anions, into a three-dimensional coordination network. The succinate anions are located on centres of inversion.

Coordination compounds of cobalt and cadmium with isobutyric acid amide

Energy Technology Data Exchange (ETDEWEB)

Tsivadze, A.Yu.; Ivanova, I.S.; Solovkina, O.A. (AN SSSR, Moscow. Inst. Obshchej i Neorganicheskoj Khimii)

1983-06-01

Coordination compounds of cobalt and cadmium with isobutyric acid amide (IBAA) of Co(NCS)/sub 2/x(IBAA)/sub 2/(H/sub 2/O)/sub 2/, CoCl/sub 2/(IBAA)/sub 4/, CoI/sub 2/(IBAA)/sub 8/(H/sub 2/O)/sub 2/, CdI/sub 2/(IBAA)/sub 2/ composition have been synthesized and characterized. Their infrared absorption spectra (200-400 cm/sup -1/), electron reflection spectra (200-750 nm) were studied. It is shown that in all compounds there are IBAA molecUles coordinated through an oxygen atom. Thiocyanogroups are coordinated through nitrogen atoms.

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

Energy Technology Data Exchange (ETDEWEB)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül

2017-12-01

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆F₂N₄S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆ClFN₄S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group$P\\bar 1$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) ųof compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) ųof compound (2). Structural analyses reveal that the title compounds are isostructural.