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Sample records for benzoyl naphthyl hydrazone

  1. Organotin(IV) complexes with 2-acetylpyridine benzoyl hydrazones: antimicrobial activity

    Energy Technology Data Exchange (ETDEWEB)

    Despaigne, Angel A.R.; Vieira, Lorena F.; Mendes, Isolda C.; Costa, Fernanda B. da; Beraldo, Heloisa, E-mail: hberaldo@ufmg.b [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Quimica; Speziali, Nivaldo L. [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Fisica

    2010-07-01

    Reaction of n-butyltin trichloride, [Bu{sup n}SnCl{sub 3}], and phenyltin trichloride, [PhSnCl{sub 3}], with 2-acetylpyridine benzoyl hydrazone (H2AcPh), 2-acetylpyridine para-chloro-benzoyl hydrazone (H2AcpClPh) and 2-acetylpyridine para-nitro-benzoyl hydrazone (H2AcpNO{sub 2}Ph) gave [Bu{sup n}Sn(2AcPh)Cl{sub 2}] (1), [Bu{sup n}Sn(2AcpClPh)Cl{sub 2}] (2), [Bu{sup n}Sn(2AcpNO{sub 2}Ph)Cl{sub 2}] (3), [PhSn(2AcPh)Cl{sub 2}] (4), [PhSn(2AcpClPh)Cl{sub 2}] (5) and [PhSn(2AcpNO{sub 2}Ph)Cl{sub 2}] (6) as products. Among the hydrazones H2AcpClPh proved to be the most active against Staphylococcus aureus and Candida albicans. Upon coordination the antibacterial activity of both tin and the hydrazones significantly increases. Complexes 2 and 5 revealed to be the most active as antimicrobial agents. (author)

  2. Synthesis, characterization and applications of polymer-metal chelates derived from poly[((4-acryloxy acetophenone)-divinylbenzene)] benzoyl hydrazone resins

    Indian Academy of Sciences (India)

    Thammisetty Ravi Sankar; K Kesavulu; Peddakotla Venkata Ramana

    2014-05-01

    4-Acryloxy acetophenone was prepared and subjected to suspension polymerization with divinylbenzene as a cross-linking agent. The resulting network polymer was ligated with benzoyl hydrazone. The functional polymer was treated with metal ions [Cu(II), Fe(II)]. The polymer-metal complexes obtained were characterized by elemental analysis, IR, 1H-NMR, solid state 13C cross-polarization magic-angle spinning (CP/MAS) NMR, electron paramagnetic resonance (EPR), thermogravimetric and scanning electron microscopy (SEM) studies. The maximum uptake efficiency for the metal ions was determined. The reusability of the polymer ligand was tested and it was shown that even after four cycles, the efficiency of the uptake was not altered.

  3. Protonation constant of salicylidene (N-benzoyl)glycyl hydrazone and its coordination behaviour towards some bivalent metal ions

    Indian Academy of Sciences (India)

    R K Lonibala; T R Rao; R K Babita Devia

    2006-07-01

    Protonation constant of an unsymmetrical Schiff base, salicylidene(N-benzoyl)glycyl hydrazone (SalBzGH), and formation constants of its complexes have been determined potentiometrically at different temperatures in aqueous dioxane medium. Complexes of SalBzGH with VO(IV), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) have been prepared. Elemental analyses, pH-metric, molar conductance, magnetic susceptibility, electronic, IR, ESR, XRD (powder) and NMR studies have been carried out to study the coordination behaviour of SalBzGH toward these metal ions. pH-metric and 1H NMR studies show the presence of two dissociable protons in the ligand. IR and NMR spectra suggest the tridentate nature of the ligand, coordinating as a uninegative species in the Mn(II) complex and as a dinegative species in all the other complexes. Presence of two different conformers of the ligand at room temperature and stabilization of a single conformer upon complex formation have been established from 1H NMR spectra of the metal-free ligand, Zn(II) and Hg(II) complexes recorded at 296 K. Electronic and ESR spectra indicate highly distorted tetragonal geometry for VO(IV) and Cu(II) complexes. XRD powder patterns of the Zn(II) complexes are indexed for an orthorhombic crystal system.

  4. A Simple Spectrophotometric Method for the Determination of Copper in Some Real, Environmental, Biological, Food and Soil Samples Using Salicylaldehyde Benzoyl Hydrazone

    Directory of Open Access Journals (Sweden)

    M. Jamaluddin Ahmed

    2012-06-01

    Full Text Available A very simple, ultra-sensitive, highly selective and non-extractive spectrophotometric method for the determination of trace amounts copper(II has been developed. Salicylaldehy debenzoyl hydrazone (SAL-BH has been proposed as a new analytical reagent for the direct non-extractive spectrophotometric determination of copper(II. SAL-BH reacts with copper in a slightly acidic (0.0001-0.005 M H2SO4 in 40% 1,4-dioxane media with copper(II to give a highly absorbent greenish yellow chelate with a molar ratio 1:1(CuII: SAL-BH The reaction is instantaneous and the maximum absorption was obtained at 404 nm and remains stable for 72 h. The average molar absorptivity and Sandell’s sensitivity were found to be 1.4×105 L mol-1 cm-1 and 5.0 ng cm-2 of copper(II, respectively. Linear calibration graphs were obtained for 0.01 – 18 mg L-1 of CuII. The detection limit and quantification limit of the reaction system were found to be 1 ng mL-1 and 10 µg L-1, respectively. A large excess of over 50 cations, anions and complexing agents (e.g., tartrate, oxalate, citrate, phosphate, thiocyanate etc. do not interfere in the determination. The method is highly selective for copper and was successfully used for the determination of copper in several standard reference materials (steels and alloys as well as in some environmental waters (portable and polluted, biological (human blood and urine, food and soil samples and solutions containing both copper(I and copper(II as well as some complex synthetic mixtures. The results of the proposed method for biological and food samples were comparable with AAS and were found to be in good agreement. The method has high precision and accuracy (s = ± 0.01 for 0.5 mg L-1.

  5. A simple spectrophotometric method for the determination of copper in some real, environmental, biological, food and soil samples using salicylaldehyde benzoyl hydrazone

    International Nuclear Information System (INIS)

    A very simple, ultra-sensitive, highly selective and non-extractive spectrophotometric method for the determination of trace amounts copper (II) has been developed. Salicylaldehyde debenzoyl hydrazone (SAL-BH) has been proposed as a new analytical reagent for the direct non-extractive spectrophotometric determination of copper (II). SAL-BH reacts with copper in a slightly acidic (0.0001-0.005 M H/sub 2/SO/sub 4/) in 40% 1,4-dioxane media with copper(lI) to give a highly absorbent greenish yellow chelate with a molar ratio 1:1(CuII: SAL-BH) The reaction is instantaneous and the maximum absorption was obtained at 404 nffi and remains stable for 72 h. The average molar absorptivity and Sandell's sensitivity were found to be 1.4x105 L mol-I cm/sup -1/ and 5.0 ng cm-2 of copper (II), respectively. Linear calibration graphs were obtained for 0.01 -18 mg L-1 of C/sup 11/. The detection limit and quantification limit of the reaction system were found to be 1 ng mL/sup -1/ and 10 micro.g L/sup -1/, respectively. A large excess of over 50 cations, anions and complexing agents (e.g., tartrate, oxalate, citrate, phosphate, thiocyanate etc.) do not interfere in the determination. The method is highly selective for copper and was successfully used for the determination of copper in several standard reference materials (steels and alloys) as well as in some environmental waters (portable and polluted), biological (human blood and urine), food and soil samples and solutions containing both copper (I) and copper( II) as well as some complex synthetic mixtures. The results of the proposed method for biological and food samples were comparable with AAS and were found to be in good agreement. The method has high precision and accuracy (s = t 0.01 for 0.5 mgL/sup -1/). (author)

  6. 查耳酮-2-羟基苯甲酰腙的超声波合成与热稳定性%Ultrasonic synthesis and thermal stability of chalcone-2-hydroxy benzoyl hydrazone

    Institute of Scientific and Technical Information of China (English)

    王燕燕; 郑长征; 王亮

    2015-01-01

    A compound of chalcone‐2‐hydroxybenzoyl hydrazone was ultrasonic synthesized through the condensation of chalcone and 2‐hydroxybenzoyl hydrazine ,and the effects of the reaction time ,the amount of solvent ,the temperature and the material ratio on the yield were discussed .Results show that under the condition of ultrasonic , the reaction time of 4. 5h , 10mL of the volume of solvent ,temperature of 75℃ and material ratio of 1∶1.2 is more ap‐propriate .The compound was characterized by elemental analysis ,infrared spectroscopy and 1 H NMR .The thermogravimetric analysis shows that the compound is stable below 190.98℃ .%以查耳酮和2‐羟基苯甲酰肼为原料,采用超声波合成查耳酮‐2‐羟基苯甲酰腙,研究反应时间、溶剂量、温度和摩尔比对收率的影响.结果表明,在超声波条件下,反应时间4.5h ,溶剂量10mL ,温度75℃和摩尔比1∶1.2较为适宜.通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征.热重分析表明标题化合物处于190.98℃以下时较为稳定.

  7. Compound list: naphthyl isothiocyanate [Open TG-GATEs

    Lifescience Database Archive (English)

    Full Text Available naphthyl isothiocyanate ANIT 00009 ftp://ftp.biosciencedbc.jp/archive/open-tggates/...LATEST/Human/in_vitro/naphthyl_isothiocyanate.Human.in_vitro.Liver.zip ftp://ftp.biosciencedbc.jp/archive/op...en-tggates/LATEST/Rat/in_vitro/naphthyl_isothiocyanate.Rat.in_vitro.Liver.zip ftp://ftp.biosciencedbc.jp/arc...hive/open-tggates/LATEST/Rat/in_vivo/Liver/Single/naphthyl_isothiocyanate.Rat.in_...vivo.Liver.Single.zip ftp://ftp.biosciencedbc.jp/archive/open-tggates/LATEST/Rat/in_vivo/Liver/Repeat/naphthyl_isothiocyanate.Rat.in_vivo.Liver.Repeat.zip ...

  8. Ground state of naphthyl cation: Singlet or triplet?

    Energy Technology Data Exchange (ETDEWEB)

    Dutta, Achintya Kumar; Vaval, Nayana, E-mail: np.vaval@ncl.res.in; Pal, Sourav, E-mail: s.pal@ncl.res.in [Physical Chemistry Division, CSIR-National Chemical Laboratory, Pune 411008 (India); Manohar, Prashant U. [Department of Chemistry, BITS Pilani, Pilani Campus (India)

    2014-03-21

    We present a benchmark theoretical investigation on the electronic structure and singlet-triplet(S-T) gap of 1- and 2-naphthyl cations using the CCSD(T) method. Our calculations reveal that the ground states of both the naphthyl cations are singlet, contrary to the results obtained by DFT/B3LYP calculations reported in previous theoretical studies. However, the triplet states obtained in the two structural isomers of naphthyl cation are completely different. The triplet state in 1-naphthyl cation is (π,σ) type, whereas in 2-naphthyl cation it is (σ,σ{sup ′}) type. The S-T gaps in naphthyl cations and the relative stability ordering of the singlet and the triplet states are highly sensitive to the basis-set quality as well as level of correlation, and demand for inclusion of perturbative triples in the coupled-cluster ansatz.

  9. Preparation of N-1 -naphthyl benzo- and N-phenyl benzo hydroxamic acids and study of their extractability towards Fe (III), Cr (VI) and U (VI)

    International Nuclear Information System (INIS)

    Two aryl hydroxamic acids were prepared; The N-phenyl benzo hydroxamic acid and the N-1- naphthyl benzohydroxamic acid the first one was prepared by the partial reduction of nitrobenzene to the β-phenyl hydroxylamine and coupling the latter with benzyl chloride. The reduction was carried out using ammonium chloride and zinc dust; this pair failed after so many attempts to give the N-1- naphthyl hydroxylamine. So the latter was prepared by using a somewhat milder reducing agent; hydrogen sulphide and ammonia gas in absolute alcohol. The two acids were obtained using the modified procedure of Tandon coupling the hydroxylamine with benzoyl chloride. The two acids were characterized by their melting points, elemental analysis, their I.R functional group frequencies and by their characteristic colour tests with vanadium (VI) and Iron (III). The acids were used for the extraction and spectrophotometric determination for iron (III), Chromium (VI), and Uranium (VI) from different molar solution, PH and from synthetic sea water. The maximum recovery of iron (III) occurred at PH 4 and PH 5 giving 92.25 and 91.25% when using N-1-naphthyl benzo hydroxamic acid and a maximum recovery of 100% at PH 5 with other acid. The maximum recovery of Chromium (VI) occurred at 3MH2SO4 of 97.50% when using N-1-naphthyl benzohydroxamic acid and a maximum of 94.25% at the same molar concentration with N-phenyl benzo hydroxamic acid. The maximum recovery for Uranium (VI) was occurred at PH 7 giving 100% when using N-1-naphthyl benzo hydroxamic acid and a maximum recovery of 85% at PH 7 and PH* with the other acid. The two reagents give sharp colour with both iron (III) and chromium (VI), so trials were carried out to compare the curves obtained with that of the original reagent i.e. Thiocynate and diphenylcarbazide, which give a smaller slope.(Author)

  10. 2-Benzoyl-4-chloroaniline thiosemicarbazone

    Directory of Open Access Journals (Sweden)

    Katlen C. T. Bandeira

    2014-06-01

    Full Text Available In the title compound, C14H13ClN4S, obtained from a reaction of 2-benzoyl-4-chloroaniline with thiosemicarbazide in ethanol, the dihedral angle between the aromatic rings is 81.31 (13°. In the crystal, the molecules are linked by three N—H...S hydrogen bonds, forming centrosymmetric rings with set-graph motif R22(8 and R22(18, and resulting in the formation of a two-dimensional network lying parallel to (010.

  11. Spectrophotometric determination of some metal ions using hydrazones

    International Nuclear Information System (INIS)

    In this research many starting materials were prepared, like methyl salicylate and salicylic acid hydrazide from which different derivatives of hydrazones were synthesized by coupling with carbonyl compounds like benzil monoxime and benzil mono hydrazone which are prepared and others like salicylaldehyde and benzoin. The hydrazones that were synthesized are salicylaldehyde salicylic acid hydrazone, benzoin salicylic acid hydrazone, benzil mono hydrazone salicylic acid hydrazone and benzil monoxime salicylic acid hydrazone. These reagents were determined by different methods, IR spectrophotometric determination, the nitrogen content method and melting point determination. These hydrazones act as ligands for determination of some metal ions by making different coloured complexes that were prepared for eight hydrazones with eight metal ions U (VI), Fe (II), Fe (III), Co (II), V (II), Mo (VI), Ni (II) and Cu (II). These complexes were determined by ultraviolet and visible spectrophotometer (UV/VIS) to detect their absorbance and wavelengths (λ max). The two hydrazones salicylaldehyde salicylic acid-hydrazone and benzoin salicylic acid hydrazone, were selected for determination of five metal ions (Fe (II), Fe (III), U (VI), Ni (II) and Cu (II)), using two micelles sodium n-dodecyl sulphate and pyridinium hexa decyl bromide mono hydrate. Their absorbance and wavelengths were detected using UV/VIS spectrophotometer. (Author)

  12. STUDY OF ANTIVIRAL ACTIVITY OF SOME HYDRAZONE PINOSTROBIN DERIVATIVES

    Directory of Open Access Journals (Sweden)

    G. K. Mukusheva

    2014-01-01

    Full Text Available New derivatives on the basis of hydrazone pinostrobin molecule were synthesized. Significant antiviral activity of received samples of new hydrazone pinstrobin derivatives was identified.

  13. 1-Benzoyl-3-(4-hydroxyphenylthiourea

    Directory of Open Access Journals (Sweden)

    Aisha A. Al-abbasi

    2010-12-01

    Full Text Available In the title compound, C14H12N2O2S, the aminophenol and the benzoyl groups adopt a syn–anti configuration with respect to the thiono C=S group across the thiourea C—N. The dihedral angle between the mean planes of the benzoyl and hydroxyphenyl rings is 36.77 (8°. The molecules are stabilized by intramolecular N—H...O hydrogen bonds. In the crystal, weak intermolecular C—H...O, O—H...S and N—H...O hydrogen bonds link the molecules into a chain along the c axis.

  14. Synthesis and Structure Elucidation of Benzoylated Deoxyfluoropyranosides

    OpenAIRE

    Esmurziev, Aslan M.; Simic, Nebojsa; Hoff, Bard Helge; Sundby, Eirik

    2010-01-01

    Benzoylated deoxyfluoropyranosides have been synthesized, starting with protected, unprotected, or fluorinated precursors. Fluorination of eight derivatives was compared using DAST and Deoxo-Fluor as reagents. Deoxo-Fluor was found to be especially useful in the fluorination of methyl 2,3,4-O-tribenzoyl -D-mannopyranoside and -D-glucopyranoside, resulting in better yields and avoiding the 1,6-methoxy migration experienced with DAST for one derivative. The two reagents gave comparable yields i...

  15. Guieranone A, a naphthyl butenone from the leaves of Guiera senegalensis with antifungal activity.

    Science.gov (United States)

    Silva, Olga; Gomes, Elsa T

    2003-03-01

    A new methoxylated naphthyl butenone, guieranone A (1), was isolated from the leaves of Guiera senegalensis. Its structure was elucidated as (2E)-1-(1,3,6,8-tetramethoxy-2-naphthyl)but-2-en-1-one, on the basis of spectroscopic data. Also isolated were two known naphthopyrones, 5-methyldihydroflavasperone (2) and 5-methylflavasperone (3). Guieranone (1) exhibited potent antifungal activity against Cladosporium cucumerinum and is the first naphthyl ketone derivative to have been isolated from the family Combretaceae. PMID:12662113

  16. 4-Amino-13-(1-naphthyl-[2,2]paracyclophane

    Directory of Open Access Journals (Sweden)

    Yudao Ma

    2008-04-01

    Full Text Available The title compound [systematic name: 12-amino-42-(1-naphthyl-1,4(1,4-dibenzenacyclohexaphane], C26H23N, was synthesized from 4-amino-13-bromo-[2,2]paracyclophane and 1-naphthaleneboronic acid in the presence of 1,4-dioxane. It is a new cyclophane-derived compound which can be regarded as a prospective ligand for asymmetric synthesis and catalysis. The benzene rings of the paracyclophane units are very slightly deformed from planarity as shallow boats.

  17. Characteristic of Schiff Base Salicylaldehyde Benzoyl Hydrazone%Schiff碱水杨醛苯甲酰腙的特性

    Institute of Scientific and Technical Information of China (English)

    鲁伊恒; 吕玉卫

    2004-01-01

    研究了Schiff碱水杨醛苯甲酰腙(简称SBH)晶体在DMSO及其DMSO-H2O的混合溶剂中的红外光谱,通过SBH氘代前后的IR对比发现,羟基氢质子与混合溶剂DMSO-H2O(3:1,V/V)产生较大的相互作用.向溶有SBH的75%DMSO-25%H2O的溶液滴加KOH发现,SBH分子上的C=O羰基基团先与KOH作用,其后与O-H羟基基团作用.

  18. Naphthyl-functionalized oligophenyls: Photophysical properties, film morphology, and amplified spontaneous emission

    Science.gov (United States)

    Ma, Lin; Wu, Zhaoxin; Lei, Ting; Yu, Yue; Yuan, Fang; Jiao, Bo; Hou, Xun

    2016-04-01

    Herein, we reported a series of deep-blue-emitting naphthyl-functionalized oligophenyls as new organic laser active materials with tunable wavelength from 385 to 410 nm in solid state. Introduction of peripheral naphthyl into the oligophenyls enabled the great sterical dimensions due to the prominent steric hindrance but not destroyed the molecular conjugation. We assumed that it would suppress the π-π stacking efficiently, driving by intermolecular interaction, to hinder crystallization in solid films. Finally, the neat films of naphthyl-functionalized oligophenyls demonstrated amorphous state compared to the polycrystalline state of oligophenyls. Thus, naphthyl-functionalized oligophenyls displayed high emission quantum yield (22-35%) in solid state neat films. In addition, these molecules possessed large oscillator strength and radiative decay rate, as predicted by the theoretical analysis. The outstanding photophysical properties and amorphous films render naphthyl-functionalized oligophenyls a new class of optical gain media in solid state.

  19. 40 CFR 721.5930 - Phenylenebis[imino (chlorotriazinyl)imino(substituted naphthyl)azo(substituted phenyl)azo, sodium...

    Science.gov (United States)

    2010-07-01

    ...)imino(substituted naphthyl)azo(substituted phenyl)azo, sodium salt (generic name). 721.5930 Section 721... Phenylenebis[imino (chlorotriazinyl)imino(substituted naphthyl)azo(substituted phenyl)azo, sodium salt (generic... identified generically as phenylenebis[imino (chlorotriazinyl)imino(substituted naphthyl)azo...

  20. Synthesis and characterization of lanthanide complexes of 1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl-phenyl ketone-2'-picolinoyl hydrazone

    International Nuclear Information System (INIS)

    The ligand, 1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl phenyl ketone 2'-picolinoyl hydrazone (HL) is prepared by condensation of 1-phenyl-3- methyl-4-benzoyl-5-pyrazolone with 2-picolinic acid hydrazide. Seven complexes of lanthanides with HL of the type [Ln(HL)3].2H2O (where Ln=trivalent lanthanides such as La, Ce, Nd, Sm, Gd, Dy and Er) have been synthesized and characterized by complexometric titration of lanthanoid ions, elemental analysis, molar conductance, IR, 1H NMR, electronic spectral studies and TGA analysis IR spectra and thermogram shows the presence of two water moieties outside the coordination sphere and are non-electrolytic in nature. The complexes appear to be nine-coordinated and ligand act as a tridentate ligand. (author)

  1. Azo-hydrazone tautomerism of aryl azo pyridone dyes

    Directory of Open Access Journals (Sweden)

    Mirković Jelena M.

    2013-01-01

    Full Text Available In the last three or four decades disperse dyes derived from pyridones (in particular azo pyridone dyes have gained in importance, and are widely used in various fields. These compounds have excellent coloration properties, and are suitable for the dyeing of polyester fabrics. Basic features of these dyes are simplicity of their synthesis by diazotation and azo coupling. They generally have high molar extinction coefficient with medium to high light and wet fastness. The absorption maxima of these dyes show their visible absorption wavelength ranging from yellow to orange, which can be attributed to poorly delocalized electrons in the pyridone ring. However, there are several dyes with deep colors such as red or violet. Pyridone dyes with alkyl and aryl groups in ortho position to azo group show 2-pyridone/2-hydroxypyridine tautomerism, while those containing OH and NHR groups conjugated with the azo group show azo-hydrazone tautomerism. Determining azo-hydrazone tautomerism could be therefore interesting, since the tautomers have different physico-chemical properties and most importantly different coloration. The literature on azo-hydrazone tautomerism, determination of equilibrium position, and investigation of substituent and solvent influence on tautomerism has been summarized in the presented review. The general conclusion is that the equilibrium between two tautomers is influenced by the structure of the compounds and by the solvents used. The tautomeric behavior patterns of the arylazo pyridone dyes in the reviewed literature has been studied using various instrumental techniques, including FT-IR, UV-vis, and NMR spectroscopy. The quantum chemical calculations related to the azo-hydrazon tautomerism have also been included. A large number of pyridone dyes exist in hydrazone form in solid state, while in solvents there is a mixture of tautomers. In addition, the X-ray single-crystal diffraction data analysis of some commercial pyridone

  2. A Three-Step Acne System Containing Solubilized Benzoyl Peroxide versus Benzoyl Peroxide/Clindamycin in Pediatric Patients with Acne

    OpenAIRE

    Eichenfield, Lawrence F.; Thiboutot, Diane; Shalita, Alan; Swinyer, Leonard; Tanghetti, Emil; Tschen, Eduardo; Parr, Lisa

    2009-01-01

    Objective. To evaluate the clinical benefit in adolescents of a three-step acne system containing solubilized benzoyl peroxide. Design. Patients in this multicenter, investigator-blind trial were randomly assigned to receive 10 weeks of treatment with either the three-step acne system for normal-to-oily skin (proprietary 2% salicylic acid cleanser twice daily + proprietary 2% salicylic acid toner once daily + solubilized 5% benzoyl peroxide gel twice daily) or with control cleanser + 5% benzo...

  3. Synthesis of 1-Benzoyl-3-aryl-4-hydroxy-4-phenylimidazolidin-2-thiones

    Institute of Scientific and Technical Information of China (English)

    曾润生; 邹建平; 穆学军; 沈琪

    2003-01-01

    l-Benzoyl-3-aryl-4-hydroxy-4-phenylimidazolidin-2-thiones can be synthesized readily from the cyclization of 1-benzoyl-3-arylthioureas with bromine-acetophenone in the presence of excess triethylamiqe.

  4. New phosphoro-thioates derived from naphthyl-methyl-imidazoline and naphthyl-ethyl-imidazoline: application in chemical radioprotection; Nouveaux phosphorothioates derives de la naphthylmethylimidazoline et de la naphthylethylimidazoline: application en radioprotection chimique

    Energy Technology Data Exchange (ETDEWEB)

    Celaries, B.; Rima, G. [Universite Paul Sabatier, Lab. d' Heterochimie Fondamentale et Appliquee, 31 - Toulouse (France); Amourette, C. [Centre de Recherches du Service de Sante des Armees, 38 - La Tronche (France); Lion, C. [Paris-7 Univ., ITODYS, 75 (France)

    2005-03-01

    New phosphoro-thioates derived from naphthyl-methyl-imidazoline and naphthyl-ethyl-imidazoline: application in chemical radioprotection. In this work, we report the radio-pharmacological study (radioprotective activity, toxicity) of new phosphoro-thioates derived from 2-(1-naphthyl-methyl)-2-imidazoline and 2-[1-(1-naphthyl)ethyl]-2-imidazoline. The radioprotective efficacy against {gamma}-rays of these organophosphorus compounds was evaluated in vivo. All these derivatives have shown a dose reduction factor between 1.5 and 1.9 which traduce their excellent radioprotective activity. These compounds should present an interest in the chemo- and radiotherapy treatments. (author)

  5. Microwave-assisted facile and rapid Friedel-Crafts benzoylation of arenes catalysed by bismuth trifluoromethanesulfonate

    DEFF Research Database (Denmark)

    Tran, Phoung Hoang; Hansen, Poul Erik; Pham, Thuy Than;

    2014-01-01

    The catalytic activity of metal triflates was investigated in Friedel–Crafts benzoylation under microwave irradiation. Friedel–Crafts benzoylation with benzoyl chloride of a variety of arenes containing electron-rich and electron-poor rings using bismuth triflate under microwave irradiation is...

  6. Naphthyl-Containing Organophosphonate Derivatives of Keggin-Type Polyoxotungstates

    Directory of Open Access Journals (Sweden)

    Nerea Andino

    2016-05-01

    Full Text Available New organophosphonate derivatives of monovacant Keggin-type polyoxotungstates that contain naphthyl groups have been synthesized and characterized in both solid state and solution. Single-crystal structural analysis shows that two phosphonate groups occupy the vacant position of the lacunary cluster unit in the isostructural compounds [N(C4H94]3[H(POC11H92(α-HBW11O39] (TBA-1 and [N(C4H94]3[H(POC11H92(α-SiW11O39] (TBA-2. Liquid-solution UV–Vis transmittance and solid-state diffuse reflectance spectroscopy studies reveal the presence of a new absorption band in the visible region, the charge transfer character of which has been further confirmed by time-dependent density functional theory (TD-DFT calculations. The latter evidence that the charge transfer process is dominated by transitions from the highest occupied molecular orbital (HOMO, localized in the aromatic ring of the organic group, to the lowest unoccupied molecular orbital (LUMO, localized in the Keggin anion. Photoluminescence studies show that the fluorescent properties of the 1-naphthylmethylphosphonate group are quenched upon its incorporation into the inorganic oxo-tungstate skeleton. The solution stability of the hybrid clusters has been evaluated by a combination of 1H-, 13C- and 31P-Nuclear Magnetic Resonance spectroscopy and Electrospray Ionization-Mass Spectrometry. The hybrid polyanion [H(POC11H92(α-HBW11O39]3− (1 herein constitutes the first structurally characterized organo-p-block containing borotungstate, and hence it confirms that this strategy for the organic functionalization of polyoxometalate clusters can be applied to new platforms belonging to the family of group-13 heteropolyoxotungstates.

  7. Group X Aldehyde Dehydrogenases of Pseudomonas aeruginosa PAO1 Degrade Hydrazones

    OpenAIRE

    Taniyama, Kosuke; Itoh, Hideomi; Takuwa, Atsushi; Sasaki, Yasuyuki; Yajima, Shunsuke; Toyofuku, Masanori; Nomura, Nobuhiko; Takaya, Naoki

    2012-01-01

    Hydrazones are natural and synthetic compounds containing a C=N-N moiety. Here we found that the opportunistic pathogen Pseudomonas aeruginosa PAO1 produced NAD+- or NADP+-dependent hydrazone dehydrogenase (HDH), which converts hydrazones to the corresponding hydrazides and acids rather than to the simple hydrolytic product aldehydes. Gene cloning indicated that the HDH is part of the group X aldehyde dehydrogenase (ALDH) family, which is distributed among bacteria, although the physiological...

  8. Infrared Spectroscopic Characterization of Calcium and Barium Hydrazone Complexes

    Directory of Open Access Journals (Sweden)

    *A. Adeniyi

    2013-06-01

    Full Text Available Hydrazones have attracted considerable interest on account of their biological activities. Introduction of calcium and barium metal ions into m- and p-nitrobenzoic hydrazones is expected to modify these biological properties for enhanced activity and versatility. The ligands were synthesized from the parent acids. The complexes have been characterized using C, H and N microanalyses and IR spectrometry. The IR spectral data of the ligands and complexes revealed bonding via the C=O and C=N groups. The suggested metal to ligand stoichiometries are: [M (m-NBHx]Cl2.yH2O, x, y = 1 and 4 for M = Ca; x, y = 2 and 3 for M = Ba respectively. [M(p-NBHx]Cl2.yH2O, x, y = 1 and 12 for M = Ca; x, y = 1 and 3 for M = Ba respectively. The structural deductions are tentative pending future X-ray structural studies.

  9. Selective determination of vanadium using N-benzoyl-N-phenylhydroxylamine

    International Nuclear Information System (INIS)

    Technique for selective spectrophotometric vanadium determination in alloys after extraction by chloroform of vanadium (5) complexes with N-benzoyl-N-phenylhydroxylamine from phosphoric acid solutions was developed. Low boundary of determination on sample dissolving ∼1 h. Effect of the nature of mineral acids and aliphatic alcohols on spectrophotometric characteristics of complexes was investigated

  10. Methyllithium-Doped Naphthyl-Containing Conjugated Microporous Polymer with Enhanced Hydrogen Storage Performance.

    Science.gov (United States)

    Xu, Dan; Sun, Lei; Li, Gang; Shang, Jin; Yang, Rui-Xia; Deng, Wei-Qiao

    2016-06-01

    Hydrogen storage is a primary challenge for using hydrogen as a fuel. With ideal hydrogen storage kinetics, the weak binding strength of hydrogen to sorbents is the key barrier to obtain decent hydrogen storage performance. Here, we reported the rational synthesis of a methyllithium-doped naphthyl-containing conjugated microporous polymer with exceptional binding strength of hydrogen to the polymer guided by theoretical simulations. Meanwhile, the experimental results showed that isosteric heat can reach up to 8.4 kJ mol(-1) and the methyllithium-doped naphthyl-containing conjugated microporous polymer exhibited an enhanced hydrogen storage performance with 150 % enhancement compared with its counterpart naphthyl-containing conjugated microporous polymer. These results indicate that this strategy provides a direction for design and synthesis of new materials that meet the US Department of Energy (DOE) hydrogen storage target. PMID:27106536

  11. Ligand substitution reactions of a phenolic quinolyl hydrazone; oxidovanadium (IV complexes

    Directory of Open Access Journals (Sweden)

    Seleem Hussein S

    2011-08-01

    Full Text Available Abstract Background Quinoline ring has therapeutic and biological activities. Quinolyl hydrazones constitute a class of excellent chelating agents. Recently, the physiological and biological activities of quinolyl hydrazones arise from their tendency to form metal chelates with transition metal ions. In this context, we have aimed to study the competency effect of a phenolic quinolyl hydrazone (H2L; primary ligand with some auxiliary ligands (Tmen, Phen or Oxine; secondary ligands towards oxidovanadium (IV ions. Results Mono- and binuclear oxidovanadium (IV - complexes were obtained from the reaction of a phenolic quinolyl hydrazone with oxidovanadium (IV- ion in absence and presence of N,N,N',N'- tetramethylethylenediamine (Tmen, 1,10-phenanthroline (Phen or 8-hydroxyquinoline (Oxine. The phenolic quinolyl hydrazone ligand behaves as monobasic bidentate (NO- donor with O- bridging. All the obtained complexes have the preferable octahedral geometry except the oxinato complex (2 which has a square pyramid geometry with no axial interaction; the only homoleptic complex in this study. Conclusion The ligand exchange (substitution/replacement reactions reflect the strong competency power of the auxiliary aromatic ligands (Phen/Oxine compared to the phenolic quinolyl hydrazone (H2L towards oxidovanadium (IV ion; (complexes 2 and 3. By contrast, in case of the more flexible aliphatic competitor (Tmen, an adduct was obtained (4. The obtained complexes reflect the strength of the ligand field towards the oxidovanadium (IV- ion; Oxine or Phen >> phenolic hydrazone (H2L > Tmen.

  12. Structural and spectroscopic investigation on a new potentially bioactive di-hydrazone containing thiophene heterocyclic rings

    Science.gov (United States)

    Nogueira, Vanessa de S.; Ramalho Freitas, Maria Clara; Cruz, Wellington S.; Ribeiro, Tatiana S.; Resende, Jackson A. L. C.; Rey, Nicolás A.

    2016-02-01

    Hydrazones and several substituted hydrazones are associated with a broad spectrum of biological activities, as well as compounds containing the thiophene ring. In this context, a novel di-hydrazone derived from 2-thiophenecarboxylic acid hydrazide was synthesized and completely characterized by elemental analysis, XRD, FT-IR, Raman and UV-Vis spectroscopies, thermogravimetry, 1H NMR, 1H-1H COSY and 1H-1H ROESY. A preliminary in silico pharmacological evaluation was also performed in order to assess the performance of the new compound regarding some molecular properties relevant for a drug's pharmacokinetics in the human body.

  13. EPR Studies on Octakis (1-Naphthyl-Methylthio) Substituted Porphyrazine Derivatives

    International Nuclear Information System (INIS)

    New porphyrazines surrounded with eight bulky and electron-rich naphthyl groups have been described, high electron density on the substituents results with a second absorption in the ultraviolet region of comparable intensity as the intense B band of porphyrazines. Characterization of octakis (1-naphthyl-methylthio) substituted porphyrazine derivatives coordinated by Co2+ and Cu2+ have been supported by EPR study. Spin-Hamiltonian parameters and line width characteristics have been obtained for both solid powder and solution forms of ion coordinated complexes. Theoretical simulations were drawn for each registered EPR spectra. Stable planar structure has been proven for both Co2+ and Cu2+ coordinated complexes one more time. Orbital energy levels for magnetic electrons were determined from EPR parameters.

  14. Physical, Thermal, and Spectroscopic Characterization of Biofield Energy Treated Methyl-2-Naphthyl Ether

    OpenAIRE

    Trivedi, Mahendra Kumar

    2015-01-01

    Methyl-2-naphthyl ether (MNE) is an organic compound and used as the primary moiety for the synthesis of several antimicrobial and anti-inflammatory agents. This study was attempted to evaluate the impact of biofield energy treatment on the physical, thermal, and spectroscopic properties of MNE. The study was carried out in two groups i.e., control and treated. The treated group was subjected to Mr. Trivedi’s biofield treatment. Afterward, the control and treated samples of MNE were eva...

  15. Structural studies of PCU-hydrazones: NMR spectroscopy, X-ray diffractions, and DFT calculations

    Science.gov (United States)

    Veljković, Jelena; Šekutor, Marina; Molčanov, Krešimir; Lo, Rabindranath; Ganguly, Bishwajit; Mlinarić-Majerski, Kata

    2011-06-01

    In this article we present a detailed structural investigation for the configurational isomers of PCU-hydrazones. The structural characterization of these hydrazones was performed using NMR spectroscopy, X-ray diffraction analysis and theoretical calculations. The single crystal X-ray structures of PCU-hydrazones 6B and 6C have been solved and used to conclusively confirm the characterization obtained via NMR spectra of a particular isomer. Nuclear magnetic shielding values calculated for 6A-C using DFT calculations were correlated with the experimentally determined chemical shifts. The computed results were found to be in good agreement with the observed 13C NMR values. The computed NMR results helped to ascertain the isomers of PCU-hydrazones 4A-C.

  16. Preparation and Physicochemical Evaluation of Benzoyl Peroxide 5% Foamable Emu oil Emulsion

    OpenAIRE

    Shatalebi; Roostaei

    2015-01-01

    Background Acne vulgaris is the most common skin disorder, characterized by the inflammation of the pilosebaceous glands. In addition to physical disfigurement, acne vulgaris may be responsible for significant emotional and physiological distress. Many medications involve in prevention and treatment of acne. Benzoyl peroxide could be a potent candidate with special formulation to treat acne. Objectives Benzoyl peroxide foamable em...

  17. Investigating the Stability of Benzoyl Peroxide in Over-the-Counter Acne Medications

    Science.gov (United States)

    Kittredge, Marina Canepa; Kittredge, Kevin W.; Sokol, Melissa S.; Sarquis, Arlyne M.; Sennet, Laura M.

    2008-01-01

    One of the most commonly used ingredients in over-the-counter acne treatments in cream, gel, and wash form is benzoyl peroxide. It is an anti-bacterial agent that kills the bacterium ("Propionibacterium acne") involved in the formation of acne. The formulation of these products is extremely difficult owing to the instability of benzoyl peroxide.…

  18. Reactions of azoalkenes derived from hydrazones of ethyl bromopyruvate with electron rich alkenes and heterocycles

    OpenAIRE

    Clarke, S.; Gilchrist, Thomas L.; Lemos, A.; G. Roberts, Tony

    1991-01-01

    Three hydrazones of ethyl bromopyruvate, the dinitrophenylhydrazone 2a, the toluene-4-sulphonylhydrazone 2b and the t-butoxycarbonylhydrazone 2c, have been reacted with a series of nucleophilic alkenes and heterocycles in the presence of sodium carbonate. Azoalkenes 3 are presumed as intermediates and adducts have been isolated. The azoalkenes derived from hydrazones 2a and 2c are found to be useful electrophiles and electrophilic dienes.

  19. The Tolerability Profile of Clindamycin 1%/Benzoyl Peroxide 5% Gel vs. Adapalene 0.1%/Benzoyl Peroxide 2.5% Gel for Facial Acne: Results of Two Randomized, Single-Blind, Split-Face Studies

    OpenAIRE

    Green, Lawrence; Cirigliano, Marcela; Gwazdauskas, Jennifer A; Gonzalez, Pablo

    2012-01-01

    Objective: To compare the first two weeks of tolerability of clindamycin/benzoyl peroxide gel versus adapalene/benzoyl peroxide gel followed by six weeks of open-label clindamycin/benzoyl peroxide gel therapy in subjects with mild-to-moderate acne who participated in two eight-week, identically designed, clinical studies. Methods: Using a split-face method, patients received both clindamycin/benzoyl peroxide gel and adapalene/benzoyl peroxide gel once daily for two weeks (allocation to the ri...

  20. Comparative study of Palladium (II using 4-Hydroxy 3, 5 dimethoxy benzaldehyde 4-hydroxy benzoyl hydrazone and Cinnamaldehyde 4-hydroxy benzoylhydrazone in presence of micellar medium by Spectrophotometry

    Directory of Open Access Journals (Sweden)

    D.Gopala Krishna,

    2010-09-01

    Full Text Available Two simple, sensitive, rapid and selective spectrophotometric methods have been developed for the determination of Palladium (II using newly synthesized reagents 4-Hdroxy3,5dimethoxy benzaldehyde-4-hydroxybenzoylhydrazone (HDMBHBH and Cinnamaldehyde 4-hydroxy benzoylhydrazone (CMHBH in presence of neutral surfactant TritonX-100-5% (micellar medium. Palladium (II forms a brown coluored water-soluble complex with HDMBHBH and CMHBH-in the pH range 1.0-6.0. The Pd (II-HDMBHBH complex shows maximum absorbance at max 373 nm in the pH range 3.0-4.0 and Pd (II-CMHBH shows at max 375 nm in thepH range 4.0-5.0. At these wavelengths (max, the complex shows maximum absorbance while the reagent blanks shows negligible absorbance. Hence, analytical studies were carried out at max 373 nm at pH 3.0 for HDMBHBH and 375 nm at pH 4.0 for CMHBH against reagent blanks. Beer's law is obeyed in the range 0.106-1.064 μg ml-1 and the optimum concentration range from ringbom plot is 0.212-0.957 g/ml of Palladium (II for both reagents. The molar absorptivity and Sandell's sensitivity for the coloured solution were found to be 7.5 x 104 L mol-1 cm-1 and 0.0015-μg. cm-2 for HDMBHBH, 6.0x104L mol-1 cm-1 , and 0.0017 -μg. cm-2 for CMHBH respectively. The interference effects of various diverse ions have been studied. Palladium (II forms 1:1 complex with HDMBHBH and CMHBH stoichiometry with stability constant 7.29 x 106 for HDMBHBH and 3.55 x 106 for CMHBH. The standard deviation in the determination of 0.638-μg ml-1 of Palladium (II is 0.003 for HDMBHBH and 0.008 for CMHBH. The Relative standard deviation is 0.71% for HDMBHBH and 2.5% for CMHBH. First and second order derivative spectroscopic methods were developed at max 422 nm and 444 nm for HDMBHBH and at 402 nm and438 nm for CMHBH respectively, for the determination of Palladium (II, which is more sensitive than the zero order method. The developed method has been employed for the determination of Palladium (II in hydrogenation catalyst samples, synthetic alloy samples and in water samples. The results are in good agreement with the certifiedvalues.

  1. Rapid detection of benzoyl peroxide in wheat flour by using Raman scattering spectroscopy

    Science.gov (United States)

    Zhao, Juan; Peng, Yankun; Chao, Kuanglin; Qin, Jianwei; Dhakal, Sagar; Xu, Tianfeng

    2015-05-01

    Benzoyl peroxide is a common flour additive that improves the whiteness of flour and the storage properties of flour products. However, benzoyl peroxide adversely affects the nutritional content of flour, and excess consumption causes nausea, dizziness, other poisoning, and serious liver damage. This study was focus on detection of the benzoyl peroxide added in wheat flour. A Raman scattering spectroscopy system was used to acquire spectral signal from sample data and identify benzoyl peroxide based on Raman spectral peak position. The optical devices consisted of Raman spectrometer and CCD camera, 785 nm laser module, optical fiber, prober, and a translation stage to develop a real-time, nondestructive detection system. Pure flour, pure benzoyl peroxide and different concentrations of benzoyl peroxide mixed with flour were prepared as three sets samples to measure the Raman spectrum. These samples were placed in the same type of petri dish to maintain a fixed distance between the Raman CCD and petri dish during spectral collection. The mixed samples were worked by pretreatment of homogenization and collected multiple sets of data of each mixture. The exposure time of this experiment was set at 0.5s. The Savitzky Golay (S-G) algorithm and polynomial curve-fitting method was applied to remove the fluorescence background from the Raman spectrum. The Raman spectral peaks at 619 cm-1, 848 cm-1, 890 cm-1, 1001 cm-1, 1234 cm-1, 1603cm-1, 1777cm-1 were identified as the Raman fingerprint of benzoyl peroxide. Based on the relationship between the Raman intensity of the most prominent peak at around 1001 cm-1 and log values of benzoyl peroxide concentrations, the chemical concentration prediction model was developed. This research demonstrated that Raman detection system could effectively and rapidly identify benzoyl peroxide adulteration in wheat flour. The experimental result is promising and the system with further modification can be applicable for more products in near

  2. 芳酰腙配体与Ni(Ⅱ)和Co(Ⅱ)配合物的水热合成与晶体结构%Hydrothermal Synthesis and Crystal Structure of Ni(Ⅱ) and Co(Ⅱ) Complexes with Hydrazone Ligand

    Institute of Scientific and Technical Information of China (English)

    郑长征; 王亮; 刘娟

    2012-01-01

    A new bidentate ON hydrazone ligand,has been designed and synthesized by benzylidene acetophenone with benzoyl hydrazine (Hbabh).Two coordination compounds,namely [M(babh)2(py)2] (M=Ni,1;Co,2; Hbabh=benzylidene acetophenone benzoyl hydrazone,py=pyridine),have been hydrothermally synthesized and characterized by analytical,IR,TG analysis and single-crystal X-ray diffraction measurements.The two compounds crystallize in the Monoclinic space group P21/n.A view of 2D sheet structure in 1 and 2 are packed alongside with each other through weak C-H...π interactions.CCDC:819582,1; 819583,2.%由苯亚甲基苯乙酮和苯甲酰肼合成一种新型双齿(O、N)酰腙配体(苯亚甲基苯乙酮苯甲酰腙).由水热法合成了两种配合物[M(babh)2(py)2](M=Ni,1;Co,2;Hbabh=苯亚甲基苯乙酮苯甲酰腙,py=吡啶),并用元素分析、红外、热重及X-射线单晶衍射对其进行了表征.晶体结构分析结果表明:两个化合物均属单斜晶系,空间群均是P21/n.化合物1和2通过分子间弱的C-H…π堆积形成二维片状超分子层.

  3. White organic light-emitting diodes with 9, 10-bis (2-naphthyl) anthracene

    Energy Technology Data Exchange (ETDEWEB)

    Guan Yunxia; Niu Lianbin [Key Laboratory of Optical Engineering, College of Physics and Information Technology, Chongqing Normal University, Chongqing 400047 (China)], E-mail: gyxybsy@126.com, E-mail: niulb03@126.com

    2009-03-01

    White organic light-emitting diodes were fabricated by 9, 10-bis (2-naphthyl) anthracene (ADN) doped with Rubrene with a structure of ITO/copper phthalocyanine (CuPc) / NPB /ADN: Rubrene /Alq{sub 3} /CsF/Mg:Ag/Ag. Multilayer organic devices using AND and Rubrene as an emitting layer produced white emissions with good chromaticity and luminous efficiency as high as 5.93 cd/A. This performance can be explained by Foerster energy transfer from the blue-emitting host to the orange-emitting dopant.

  4. (Z)-4-(2-Naphthyl­amino)­pent-3-en-2-one

    OpenAIRE

    Harrad, Mohamed Anoir; Boualy, Brahim; Oudahmane, Abdelghani; Avignant, Daniel; Rizzoli, Corrado

    2011-01-01

    The title compound, C15H15NO, which was synthesized under solvent-free conditions by the reaction of acetoacetone and 2-naphthyl­amine, adopts a Z conformation about the C=C bond. The enamine–ketone fragment is approximately planar [maximum deviation = 0.026 (3) Å] and forms a dihedral angle of 39.78 (3)° with the naphthalene ring system. An intra­molecular N—H⋯O hydrogen bond is observed.

  5. Synthesis, spectroscopic characterizations, crystal structures and DFT studies of nalidixic acid carbonyl hydrazones derivatives

    Science.gov (United States)

    Bergamini, F. R. G.; Ribeiro, M. A.; Lancellotti, M.; Machado, D.; Miranda, P. C. M. L.; Cuin, A.; Formiga, A. L. B.; Corbi, P. P.

    2016-09-01

    This article describes the synthesis and characterization of the 1-ethyl-7-methyl-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carbohydrazide (hzd) and six carbonyl hydrazones derivatives of the nalidixic with 1H-pyrrol-2-ylmethylidene (hpyrr), 1H-imidazol-2-ylmethylidene (h2imi), pyridin-2-ylmethylidene (h2py), pyridin-3-ylmethylidene (h3py), pyridin-4-ylmethylidene(h4py) and (2-hydroxyphenyl)methylidene (hsali). The carbonyl hydrazones were characterized by elemental and ESI-QTOF-MS analyses, IR and detailed NMR spectroscopic measurements. The 2D NMR experiments allowed the unambiguous assignment of the hydrogen, carbon and nitrogen atoms, which have not been reported for nalidixic acid carbonyl hydrazone derivatives so far. Crystal structures of hzd and the new carbonyl hydrazones h2imi, hpyrr and h3py were determined by X-ray diffraction studies. Although the synthesis of hzd was reported decades ago, the hzd crystal structure have not been reported yet. Geometric optimizations of all the characterized structures were performed with the aid of DFT studies. Despite the fact that the hydrazones with 2-pyridine carboxylic acid (h2py) and salicyl aldehyde (hsali) were already reported by literature, a detailed spectroscopic study followed by DFT studies are also reported for such compounds in this manuscript. Antimicrobial studies of the compounds are also presented.

  6. Investigation of Keto-enol Tautomers during the Synthesis of Aryl-bis (2-hydroxy-1-naphthyl)Methanes

    Indian Academy of Sciences (India)

    Papia Dutta; Mrinal Saikia; Rashmi Jyoti Das; Ruli Borah

    2014-11-01

    This study investigated the existence of keto-enol tautomers for the first time during the synthesis of aryl-bis(2-hydroxy-1-naphthyl)methane from 2-naphthol and -tolualdehyde or 4-chlorobenzaldehyde in methanol using CuSO4.5H2O as catalyst under reflux condition. The exclusive formation of aryl-bis(2-hydroxy-1-naphthyl)methaneswas observed in dichloromethane at room temperature in the presence of BF3.OEt2/AcOH as catalyst. The keto productswere isolated and characterized by 1HNMR, 13C NMR, COSY and DEPTspectra.

  7. Ruthenium(II) hydrazone Schiff base complexes: Synthesis, spectral study and catalytic applications

    Science.gov (United States)

    Manikandan, R.; Viswanathamurthi, P.; Muthukumar, M.

    2011-12-01

    Ruthenium(II) hydrazone Schiff base complexes of the type [RuCl(CO)(B)(L)] (were B = PPh 3, AsPh 3 or Py; L = hydrazone Schiff base ligands) were synthesized from the reactions of hydrazone Schiff base ligand (obtained from isonicotinoylhydrazide and different hydroxy aldehydes) with [RuHCl(CO)(EPh 3) 2(B)] (where E = P or As; B = PPh 3, AsPh 3 or Py) in 1:1 molar ratio. All the new complexes have been characterized by analytical and spectral (FT-IR, electronic, 1H, 13C and 31P NMR) data. They have been tentatively assigned an octahedral structure. The synthesized complexes have exhibited catalytic activity for oxidation of benzyl alcohol to benzaldehyde and cyclohexanol to cyclohexanone in the presence of N-methyl morpholine N-oxide (NMO) as co-oxidant. They were also found to catalyze the transfer hydrogenation of aliphatic and aromatic ketones to alcohols in KOH/Isopropanol.

  8. Supramolecular arrangement in mono and bi-camphor acyl hydrazones: A structural study

    Science.gov (United States)

    Galvão, Adelino M.; Carvalho, M. Fernanda N. N.; Ferreira, Ana S. D.

    2016-03-01

    New acyl hydrazones were synthesized by condensation with camphorquinone aiming at extending the range of applications of the biologically active camphor compounds and structural studies by XRD, 1H-NMR and IR were used in conjunction with advanced computational methodologies to understand the new structural chemistry enabled by the conjugation of the camphor ketone group to the hydrazone Ndbnd C double bond. In particular, were analysed supramolecular arrangements either by hydrogen bonding to water molecules or electrostatic interactions with non protic solvents. The relative stability of all conformers (E/Z) prompted by the hydrazone bond was addressed by state of the art methods such as CR-CCSD(T) and their inter-conversion in both S0 and S1 by CR-EOM-CCSD(T).

  9. Iridium mediated phenolic O-H activation and cyclometalation of 2-(naphthyl-1'-azo)-4-methylphenol - Formation of organoiridium complexes

    Indian Academy of Sciences (India)

    Rama Acharyya; Shie-Ming Peng; Gene-Hsiang Lee; Samaresh Bhattacharya

    2009-07-01

    Reaction of 2-(naphthyl-1'-azo)-4-methylphenol with [Ir(PPh3)3Cl] in refluxing ethanol in the presence of a base (NEt3) affords an organoiridium complex of type [Ir(PPh3)2(L)(H)], where L represents the coordinated 2-(naphthyl-1'-azo)-4-methylphenolate ligand. A similar reaction carried out in toluene affords the [Ir(PPh3)2(L)(H)] complex along with a similar complex of type [Ir(PPh3)2(L)Cl]. Structures of both the [Ir(PPh3)2(L)(H)] and [Ir(PPh3)2(L)Cl] complexes have been determined by X-ray crystallography. In both the complexes, 2-(naphthyl-1'-azo)-4-methylphenol is coordinated to iridium, via C-H activation at the 2' position of the naphthyl ring, as a dianionic tridentate C, N, O-donor and the two triphenylphosphines are trans. The organoiridium complexes show intense MLCT transitions in the visible region. Cyclic voltammetry on the [Ir(PPh3)2(L)(H)] and [Ir(PPh3)2(L)Cl] complexes shows a reversible Ir(III)-Ir(IV) oxidation respectively at 0.55 and 0.73 V vs SCE. An irreversible oxidation of the coordinated 2-(naphthyl-1'-azo)-4-methylphenolate ligand is observed above 1.0 V vs SCE and an irreversible reduction of the same is observed near -1.0 V vs SCE.

  10. Surface diffusion and surface crystal growth of tris-naphthyl benzene glasses

    Science.gov (United States)

    Ruan, Shigang; Zhang, Wei; Sun, Ye; Ediger, M. D.; Yu, Lian

    2016-08-01

    Surface self-diffusion coefficients of α,α,β-tris-naphthyl benzene (TNB) glasses have been measured using the method of surface grating decay. For 1000 nm wavelength gratings, the decay occurs by viscous flow at temperatures above Tg + 15 K, where Tg is the glass transition temperature (347 K), and by surface diffusion at lower temperatures. Surface diffusion of TNB is vastly faster than bulk diffusion, by a factor of 107 at Tg. Comparing TNB with other molecular glasses, each evaluated at its own Tg, we find that surface diffusion has a greater system-to-system variation than bulk diffusion, slowing down with increasing molecular size and intermolecular hydrogen bonding. Experimentally determined surface diffusion coefficients are in reasonable agreement with those from simulations and theoretical predictions. TNB and other molecular glasses show fast crystal growth on the free surface and the growth velocity is nearly proportional to the surface diffusion coefficient, indicating that the process is supported by surface mobility.

  11. Pulse radiolysis of 1,2-di(α-naphthyl)ethane in deoxygenated methanol and tetrahydrofuran

    International Nuclear Information System (INIS)

    Pulse radiolysis of 1,2-di(α-naphthyl)ethane (1,2-DNE) was performed in deoxygenated pure methanol and tetrahydrofuran (THF). Absorption spectra and kinetics of 1,2-DNE- in both solvents are presented. In methanol 1,2-DNE- is formed and decays by a second order reaction. No cleavage of benzylic C-C bond occurs as has been observed in the presence of alkali metals in ethers. Hence, it can be concluded that the assistance of the metal cations is necessary for the reductive bond splitting process. For comparison, 1-bromomethylnaphthalene (Br-MN) and 1,2-diphenylethane (1,2-DPE) were investigated in deoxygenated methanol and results are given. Probable reaction mechanisms are presented. (author)

  12. Synthesis, Characterization, and Modeling of Naphthyl-Terminated sp Carbon Chains: Dinaphthylpolyynes

    CERN Document Server

    Cataldo, Franco; Cinquanta, Eugenio; Castelli, Ivano Eligio; Manini, Nicola; Onida, Giovanni; Milani, Paolo; 10.1021/jp104863v

    2010-01-01

    We report a combined study on the synthesis, spectroscopic characterization and theoretical modelling of a series of {\\alpha},{\\omega}-dinaphthylpolyynes. We synthesized this family of naphtyl-terminated sp carbon chains by reacting diiodoacetylene and 1-ethynylnaphthalene under the Cadiot-Chodkiewicz reaction conditions. By means of liquid chromatography (HPLC), we separated the products and recorded their electronic absorption spectra, which enabled us to identify the complete series of dinaphthylpolyynes Ar-C2n-Ar (with Ar = naphthyl group and n = number of acetilenic units) with n ranging from 2 to 6. The longest wavelength transition (LWT) in the electronic spectra of the dinaphthylpolyynes red shifts linearly with n away from the LWT of the bare termination. This result is also supported by DFT-LDA simulations. Finally, we probed the stability of the dinaphthylpolyynes in a solid-state precipitate by Fourier-transform infrared spectroscopy and by differential scanning calorimetry (DSC).

  13. A 6% Benzoyl Peroxide Foaming Cloth Cleanser Used in the Treatment of Acne Vulgaris: Aesthetic Characteristics, Patient Preference Considerations, and Impact on Compliance with Treatment

    OpenAIRE

    Del Rosso, James Q.

    2009-01-01

    Objective: The study was conducted to evaluate the product attributes of a new benzoyl peroxide-containing foaming cloth cleanser and to compare the overall patient satisfaction of this product with two currently available benzoyl peroxide acne products (6% benzoyl peroxide cleanser and 4% benzoyl peroxide wash). Design: This was a randomized, single-blind study. Setting: Two clinical trial sites. Participants: Male and female subjects (N=193) aged 17 to 30 years with a history of acne vulgar...

  14. Peroxo complexes of uranium(VI) with N-benzoyl urea and related ligands: synthesis, characterization and antifungal activity

    International Nuclear Information System (INIS)

    The peroxouranium(VI) complexes containing N-benzoyl urea and related ligands having composition (UO(O2)L-L(NO3)2).H2O (where L-L=N-benzoyl urea (NBU), N-benzoyl thiourea (NBT). N-benzoyl hydrazine (NBHz) and N-benzoyl hydroxylamine (NBHA)) are reported. The synthesized complexes have been characterized by various physico-chemical techniques, viz, elemental analysis, molar conductivity, magnetic susceptibility measurements, infra red, electronic, mass spectral and TGA/DTA studies. These studies revealed that the synthesized complexes are non-electrolytic and diamagnetic in nature. The ligands are bound to metal in a bidentate mode. Thermal analysis results provide conclusive evidence for the presence of water molecule in the complexes. Mass spectra confirm the molecular mass of the complexes. Antifungal activity of complexes revealed enhanced activity of complexes as compared to corresponding ligands. (author)

  15. Photoluminescence of (quinap)tricarbonylrhenium(I) chloride with QUINAP=1-(2-diphenylphosphino-1-naphthyl)isoquinoline

    Science.gov (United States)

    Kunkely, Horst; Vogler, Arnd

    2002-05-01

    The complex (quinap)Re I(CO) 3Cl, with quinap =1-(2-diphenylphosphino-1-naphthyl)isoquinoline, shows a luminescence at λ max=582 nm with φ=0.12 and τ=1.4 μs in solution (e.g., CH 2Cl 2) at r.t. It is suggested that this emission originates from a Re I to quinap metal-to-ligand charge transfer triplet.

  16. The importance of the rotor in hydrazone-based molecular switches

    Directory of Open Access Journals (Sweden)

    Xin Su

    2012-06-01

    Full Text Available The pH-activated E/Z isomerization of a series of hydrazone-based systems having different functional groups as part of the rotor (R = COMe, CN, Me, H, was studied. The switching efficiency of these systems was compared to that of a hydrazone-based molecular switch (R = COOEt whose E/Z isomerization is fully reversible. It was found that the nature of the R group is critical for efficient switching to occur; the R group should be a moderate H-bond acceptor in order to (i provide enough driving force for the rotor to move upon protonation, and (ii stabilize the obtained Z configuration, to achieve full conversion.

  17. SYNTHESIS AND BIOLOGICAL EVALUATION OF SOME PHENYL ACETIC ACID HYDRAZONE DERIVATIVES

    Directory of Open Access Journals (Sweden)

    Jadon Gunjan

    2011-11-01

    Full Text Available These products are the result of further operation after the derivation of three hydrazones derivative compounds-N'-(4-Chlorobenzylidene-2-phenylacetohydrazideN'-(2chlorobenzylidene-2-phenylacetohydrazideN'-(3, 4, 5-trimethoxybenzylidene-2-phenylacetohydrazideN'-(furan-2-ylmethylene-2-phenylacetohydrazideN'-(3, 4, 5-Trimethoxybenzylidene-2-phenylacetohydrazideN'-(1-(4-hydroxyhenyl ethylidene-2-phenylacetohydrazideThese make a considerable interest in process development of novel compounds with anticonvulsant, antidepressant, analgesic, and anti-inflammatory, anti platelet, anti malarial, antimicrobial, antimycobacterial, antitumoral, vasodilator, and antiviral and antis chistosomiasis activities. These all three compounds evaluated their biological activities. These observations have been guiding for the development of new hydrazones that possess varied biological activities.

  18. Antibacterial, antifungal and antimycobacterial activities of some pyrazoline, hydrazone and chalcone derivatives.

    Science.gov (United States)

    Evranos-Aksöz, Begüm; Onurdağ, Fatma Kaynak; Özgacar, Selda Özgen

    2015-07-01

    Twenty-seven previously reported chalcones and their pyrazoline and hydrazone derivatives as well as two further chalcones have been screened for their antimicrobial, antifungal and antimycobacterial activities against standard microbial strains and drug resistant isolates. The minimum inhibitory concentration (MIC) value of each compound was determined by a two-fold serial microdilution technique. The compounds were found to possess a broad spectrum of antimicrobial activities with MIC values of 8-128 μg/mL. One compound [(E)-1-(4-hydroxyphenyl)-3-p-tolylprop-2-en-1-one] had equal activity with gentamycin (8 μg/mL) against Enterococcus faecalis. Chalcones were found to be more active than their hydrazone and 2-pyrazoline derivatives against Staphylococcus aureus ATCC 29213 and E. faecalis ATCC 29212. PMID:26372110

  19. Spectroscopic and theoretical study of the o-vanillin hydrazone of the mycobactericidal drug isoniazid

    Science.gov (United States)

    González-Baró, Ana C.; Pis-Diez, Reinaldo; Parajón-Costa, Beatriz S.; Rey, Nicolás A.

    2012-01-01

    A complete and detailed study of the hydrazone obtained from condensation of antituberculous isoniazid (hydrazide of the isonicotinic acid, INH) and o-vanillin (2-hydroxy-3-methoxybenzaldehyde, o-HVa) is performed. It includes structural and spectroscopic analyses, comparing experimental and theoretical results. The compound was obtained as a chloride of the pyridinic salt (INHOVA +Cl -) but it will be referred as INHOVA for the sake of simplicity. The conformational space was searched and optimized geometries were determined both in gas phase and including solvent effects. Vibrational (IR and Raman), electronic and NMR spectra were registered and assigned with the help of computational methods based on the Density Functional Theory. Isoniazid hydrazones are good candidates for therapeutic agents against tuberculosis with conserved efficiency and lower toxicity and resistance than parent INH.

  20. Studies on hydrazone and azine derivatives of bis(indenyl)-titanium(IV) and -zirconium(IV)

    International Nuclear Information System (INIS)

    Hydrazone and azine derivatives of bis(indenyl)-titanium(IV) and -zirconium(IV) of the types M(C6H4OCR':NNHR)(C9H7)2Cl and M(C6H4OCR'':NN:CR''OC6H4)(C9H7)2, where M = Ti or Zr, R = H or CH3, R' = H.C6H5 or C6H3(NO2)2 and R'' = H or CH3, have been synthesized by the reaction of bis(indenyl)titanium(IV)/zirconium(IV) dichloride and appropriate hydrazone or azine in equimolar ratio in refluxing tetrahydrofuran. The products have been characterized by chemical analyses, electrical conductance, IR, 1H NMR and electronic spectral studies. (author)

  1. Integrated kinetic studies and computational analysis on naphthyl chalcones as mushroom tyrosinase inhibitors.

    Science.gov (United States)

    Radhakrishnan, Sini; Shimmon, Ronald; Conn, Costa; Baker, Anthony

    2015-10-01

    Melanin helps to protect skin from the damaging ultraviolet radiation of the sun. Tyrosinase, the key enzyme in melanogenesis is responsible for coloration of skin, hair and eyes. This enzyme is considered to have a critical role in governing the quality and economics of fruits and vegetables, as tyrosinase activity can lead to spoilage through browning. Development of tyrosinase inhibitors is a promising approach to combat hyperpigmentation conditions like ephelides, lentigo, freckles and post-inflammatory hyperpigmentation. In the present study, we have used a docking algorithm to simulate binding between tyrosinase and hydroxy-substituted naphthyl chalcone oxime compounds and studied the inhibition of tyrosinase. The results of virtual screening studies indicated that the estimated free energy of binding of all the docked ligands ranged between -19.29 and -9.12 kcal/mol. Two of the oximes synthesized were identified as competitive tyrosinase inhibitors and were found to be twice as potent as the control kojic acid with their IC50 values of 12.22 μM and 19.45 μM, respectively. This strategy of integrating experimental and virtual screening methods could give better insights to explore potent depigmentation agents. PMID:26318997

  2. Use of Hydrazone Derivates as Inhibitors for the Corrosion of Nickel in Hydrochloric Acid Solution

    OpenAIRE

    A.S. Fouda, H. A. Mostafa, S. E. Ghazy and S. A. El- Farah

    2007-01-01

    The influence of hydrazone derivatives on the corrosion of nickel in 2 mol L-1 hydrochloric acid solution has been studied using weight loss and galvanostatic polarization techniques. In general, at constant acid concentration, the inhibition efficiency increases with increasing the inhibitor concentration and decreases with increasing temperature. Polarization studies indicate that the compounds act as mixed- type inhibitors. The addition of iodide ions enhances the inhibition efficiency to ...

  3. Optimized protocol for the radioiodination of hydrazone-type polymer drug delivery systems

    Czech Academy of Sciences Publication Activity Database

    Sedláček, Ondřej; Kučka, Jan; Hrubý, Martin

    2015-01-01

    Roč. 95, January (2015), s. 129-134. ISSN 0969-8043 R&D Projects: GA MPO FR-TI4/625; GA ČR GAP304/12/0950; GA MŠk(CZ) LH14079 Grant ostatní: AV ČR(CZ) M200501201 Institutional support: RVO:61389013 Keywords : doxorubicin * hydrazone * polymer conjugate Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.231, year: 2014

  4. Caffeine-hydrazones as anticancer agents with pronounced selectivity toward T-lymphoblastic leukaemia cells

    Czech Academy of Sciences Publication Activity Database

    Kaplánek, R.; Jakubek, M.; Rak, J.; Kejik, Z.; Havlík, M.; Dolenský, B.; Frydrych, I.; Hajduch, M.; Kolář, M.; Bogdanová, K.; Králová, Jarmila; Dzubak, P.; Král, V.

    2015-01-01

    Roč. 60, Jun (2015), s. 19-29. ISSN 0045-2068 Grant ostatní: GA MŠk(CZ) EE2.3.30.0060; GA MŠk CZ.1.07/2.3.00/30.0041; GA MŠk(CZ) LO1304 Institutional support: RVO:68378050 Keywords : Anticancer agents * Cancer treatment * Caffeine-hydrazones * Leukaemia * Selectivity Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.152, year: 2014

  5. Synthesis, Antifungal Activities and Qualitative Structure Activity Relationship of Carabrone Hydrazone Derivatives as Potential Antifungal Agents

    OpenAIRE

    Hao Wang; Shuang-Xi Ren; Ze-Yu He; De-Long Wang; Xiao-Nan Yan; Jun-Tao Feng; Xing Zhang

    2014-01-01

    Aimed at developing novel fungicides for relieving the ever-increasing pressure of agricultural production caused by phytopathogenic fungi, 28 new hydrazone derivatives of carabrone, a natural bioactive sesquisterpene, in three types were designed, synthesized and their antifungal activities against Botrytis cinerea and Colletotrichum lagenarium were evaluated. The result revealed that all the derivatives synthesized exhibited considerable antifungal activities in vitro and in vivo, which l...

  6. New benzoyl urea derivatives as novel NR2B selective NMDA receptor antagonists.

    Science.gov (United States)

    Borza, I; Greiner, I; Kolok, S; Galgóczy, K; Ignácz-Szendrei, Gy; Horváth, Cs; Farkas, S; Gáti, T; Háda, V; Domány, Gy

    2006-09-01

    A novel series of benzoyl urea derivatives was prepared and identified as NR2B selective NMDA receptor antagonists. The influence of the substitution of the piperidine ring on the biological activity of the compounds was studied. Compound 9 was active in the formalin test in mice. PMID:17020160

  7. Investigation of the decomposition reaction and dust explosion characteristics of crystalline benzoyl peroxides

    Energy Technology Data Exchange (ETDEWEB)

    Lu, K.-T. [Department of Applied Chemistry and Materials Science, Chung Cheng Institute of Technology, National Defense University, Taoyuan 33509, Taiwan (China)], E-mail: ktlu@ndu.edu.tw; Chen, T.-C. [Department of Applied Chemistry and Materials Science, Chung Cheng Institute of Technology, National Defense University, Taoyuan 33509, Taiwan (China); Hu, K.-H. [Department of Occupational Safety and Health, Jen-Teh Junior College of Medicine, Nursing and Management, Miaoli, Taiwan (China)

    2009-01-15

    The benzoyl peroxide (BPO) is widely used in the chemical industry. Many catastrophes have been caused by its thermal instability or reactive incompatibility in storage or thermal decomposition reaction. Thus, its hazard characteristics have to be clearly identified. First of all, the differential scanning calorimeter (DSC) is used to measure the heat of decomposition reaction, which can contribute to understanding the reaction characteristics of benzoyl peroxide. The accelerating rate calorimeter (ARC) is used to measure the rates of temperature and pressure rises of decomposition reaction, and then the kinetics parameters are estimated. Furthermore, the MIKE 3 apparatus and the 20-l-Apparatus are used to measure and analyze the dust explosion characteristics of benzoyl peroxide under room temperature and atmospheric pressure. Finally, Semenov's thermal explosion theory is applied to investigate the critical runaway condition and the stability criterion of decomposition reaction, and to build the relationship of critical temperature, convective heat transfer coefficient, heat transfer surface area and ambient temperature. These results contribute to improving the safety in the reaction, transportation and storage processes of benzoyl peroxide.

  8. A study of intracellular iron metabolism using pyridoxal isonicotinoyl hydrazone and other synthetic chelating agents

    International Nuclear Information System (INIS)

    Rabbit reticulocytes with a high level of non-heme radioiron induced by preincubation with isonicotinic acid hydrazide and transferrin-bound 59Fe, were reincubated with various synthetic chelating agents and the amount of radioiron released from the cells was determined. Some substances, especially derivatives of pyridoxal or 2-hydroxybenzaldehyde and isonicotinic acid hydrazide or benzhydrazide, were found to mobilize significantly iron from 59Fe-labelled reticulocytes. Iron mobilizaiton from reticulocytes by pyridoxal isonicotinoyl hydrazone requires ATP to be produced by cells and is completely blocked by low temperatute (40C). Although the effect of desferrioxamine is also prevented by low temperature, modest iron mobilization due to this chelator seems to occur independently of ATP production in reticulocytes. Pyridoxal isonicotinoyl hydrazone mobilized iron mainly from mitochondria and in part also from ferritin. Although 2,2'-bipyridine seems to enter reticulocyte mitochondria and bind iron there, this chelator is not able to relaease iron either from mitochondria or from the cells. Reticulocytes with a high level of non-heme radioiron are envisaged as a useful system for testing biological effectiveness of various iron chelators. Pyridoxal isonicotinoyl hydrazone was shown to be an effective in vivo chelator since its adminstration to mice decreased 59Fe radioactivity in liver, spleen and kidney. (Auth.)

  9. Hydrazone based molecular glasses for solid-state dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Biscarbazole and terthiophene based molecular glasses with hydrazone functional goups (named respectively 2CzMPH and 3TDPH) have been synthesized and the thermal, optical and electrochemical properties have been studied. Differential scanning calorimetry characterizations confirm the metastable amorphous properties of these molecules with glass transition temperatures at 80 deg. C for the 3TDPH and 93 deg. C for the 2CzMPH. Their electrochemical properties have been studied and showed the effect of the conjugated hydrazone groups on the electronic delocalization of the structures. The concept of solid state dye-sensitized solar cells using hydrazone based molecular glasses has been verified with the elaboration of a SnO2: F/nc-TiO2/Ru-dye/2CzMPH /Au devices. Under full sunlight (98 mW/cm2, air mass 1.5) the I-V characterization of the device give a short circuit photocurrents Isc = 0.42 mA/cm2, open circuit voltage Voc = 500 mV with a fill factor of 0.35

  10. Kinetics and Mechanistic Study of Permanganate Oxidation of Fluorenone Hydrazone in Alkaline Medium

    Directory of Open Access Journals (Sweden)

    Ahmed Fawzy

    2016-01-01

    Full Text Available The oxidation kinetics of fluorenone hydrazone (FH using potassium permanganate in alkaline medium were measured at a constant ionic strength of 0.1 mol dm−3 and at 25°C using UV/VIS spectrophotometer. A first-order kinetics has been monitored in the reaction of FH with respect to [permanganate]. Less-than-unit order dependence of the reaction on [FH] and [OH−] was revealed. No pronounced effect on the reaction rate by increasing ionic strength was recorded. Intervention of free radicals was observed in the reaction. The reaction mechanism describing the kinetic results was illustrated which involves formation of 1 : 1 intermediate complex between fluorenone hydrazones and the active species of permanganate. 9H-Fluorenone as the corresponding ketone was found to be the final oxidation product of fluorenone hydrazone as confirmed by GC/MS analysis and FT-IR spectroscopy. The expression rate law for the oxidation reaction was deduced. The reaction constants and mechanism have been evaluated. The activation parameters associated with the rate-limiting step of the reaction, along with the thermodynamic quantities of the equilibrium constants, have been calculated and discussed.

  11. Diastereoselective addition of Grignard reagents to α-epoxy N-sulfonyl hydrazones

    Science.gov (United States)

    Uteuliyev, Maulen M.; Nguyen, Thien T.; Coltart, Don M.

    2015-12-01

    The α-alkylation of ketones and their derivatives by the addition of their corresponding enolates to alkyl halides is a fundamental synthetic transformation, but its utility is limited because the key bond-forming step proceeds in a bimolecular nucleophilic substitution fashion. Here we describe how an umpolung strategy that involves the addition of Grignard reagents to α-epoxy N-sulfonyl hydrazones—directed by the alkoxide of the 1-azo-3-alkoxy propenes formed in situ via base-induced ring opening of the epoxide—leads to the syn-selective production of α-alkyl-β-hydroxy N-sulfonyl hydrazones with α-quaternary centres. This transformation is remarkable in its ability to incorporate an unprecedented range of carbon-based substituents, which include primary, secondary and tertiary alkyl, as well as alkenyl, aryl, allenyl and alkynyl groups. Subsequent hydrolysis of the β-hydroxy N-sulfonyl hydrazone products produces the corresponding β-hydroxy ketones. In addition to hydrolysis, the hydrazone products are poised to undergo numerous different known synthetic transformations via well-established chemistry, which would provide access to a wide array of useful structures.

  12. Photochromism of quinolylhydrazones. III. The mechanism of isomerization of the photocolored α-quinolylimino-(Z)-hydrazone to the α-quinolylamino-(E)-hydrazone

    International Nuclear Information System (INIS)

    The kinetics and mechanism of the thermal decay of the photocolored form 1a of salicylaldehyde 2-quinolylhydrazone are reported. Two isomerization reactions, viz., α-imino- to α-aminoquinoline and Z → E hydrazone, are involved. The first conversion occurs via an intramolecular transfer of the phenolic hydrogen to the α-imino group. This is deduced on the basis of medium effect, concentration effect, and base inhibition studies. The decay of the 8-nitro colored form confirms this and implicates the quinoline NH as the source of the phenolic hydrogen of the uncolored form. The overall deuterium isotope effect of 1.84 denotes the non-rate-determining nature of the participation of the OH and NH. Since plots of the logarithm of the decay rate constant k vs. solvent Z or E/sub T/ values show linear relationship and large negative ΔS values accompany the decay process, a rotation mechanism is postulated for the Z→ E hydrazone isomerization. Also, acid catalysis substantiates the mechanistic scheme proposed for the decay process. (U.S.)

  13. ER stress contributes to alpha-naphthyl isothiocyanate-induced liver injury with cholestasis in mice.

    Science.gov (United States)

    Yao, Xiaomin; Li, Yue; Cheng, Xiaoyan; Li, Hongwei

    2016-06-01

    Endoplasmic reticulum (ER) stress is involved in the development of several liver diseases and tumors. This study investigated the underlying mechanisms of α-naphthyl isothiocyanate (ANIT)-induced liver injury with cholestasis in mice and found ER stress contributes to the injury. All animals were randomly divided into three groups. In the ANIT-intoxicated group, mice were intragastrically given 100mg/kg ANIT (dissolved in corn oil), while the other groups received an equal volume of vehicle as control. After 24 and 48h of ANIT administration, blood samples and liver tissues of all animals were collected for serum biochemistry and hepatic histopathological examinations to evaluate liver injuries with cholestasis. Hepatocellular apoptosis was assessed by the terminal deoxynucleotidyl transferase dUTP nick-end labeling (TUNEL) assay. The expression of hepatic ER stress-related markers was determined by real-time PCR, immunohistochemical assay and Western blot. ANIT was found to significantly induce liver injury with cholestasis compared with control mice as evidenced by the increase of serum transaminases and total bilirubin (TBil), and histopathological changes in mice. ANIT remarkably induced hepatocellular apoptosis, upregulated the expression of caspase-9 and cytochrome c, and inhibited the gene and protein expression of proliferating cell nuclear antigen (PCNA). The gene expression of ER stress-related markers, including glucose-regulated protein 78 (GRP78), protein kinase R-like ER kinase (PERK), eukaryotic initiation factor 2α (eIF2α), inositol requiring enzyme-1α (IRE-1α) and activating transcription factor 6 (ATF6) was upregulated by ANIT in mice. ANIT also upregulated the protein expression of GRP78 and activated the phosphorylation of IRE1. These results suggested that ANIT induced liver injury with cholestasis partly due to its ability to activate the ER stress pathway. PMID:27173049

  14. Microwave assisted synthesis of some novel Flurbiprofen hydrazide- hydrazones as anti-HCV NS5B and anticancer agents

    Directory of Open Access Journals (Sweden)

    Sevil Aydın

    2013-01-01

    Full Text Available The synthesis of a new series of flurbiprofen hydrazide-hydrazones using microwave assisted reactions is described. Substituted aldehydes were condensed with flurbiprofen hydrazide by microwave irradiation to corresponding hydrazones. Synthesis of N’-[(4-bromothiophen-2-ylmethylidene]-2-(2-fluorobiphenyl-4-yl propanehydrazide (3o employing microwave assisted process resulted in higher yields, in faster time and with less chemical waste compared to traditional techniques. (2-fluorobiphenyl-4-yl-N’-(phenylmethylidenepropanehydrazide (3p andN’-[(2-chloro-6-fluorophenyl methylidene]-2-(2-fluorobiphenyl-4-ylpropanehydrazide (3s inhibited the growth of a leukemia cancercell line HL-60 (TB by 66.37% and an ovarian cancer cell line OVCAR-4 by 77.34% (singledose, 10μM, respectively at the National Cancer Institute (NCI, but had no significant ef-fect on a panel of sixty human tumor cell lines. Flurbiprofen hydrazide-hydrazones were weak inhibitors of hepatitis C virus NS5B polymerase activity with N’-[(5-ethylfuran-2-ylmethylidene]-2-(2-fluorobiphenyl-4-ylpropanehydrazide (3m being the most active of this series. Binding mode investigations of compound 3m suggested that allosteric pocket (AP-B may be the potential binding site for flurbiprofen hydrazones and these results will alsoassist in further derivatization of 3m using the green chemistry approach and improve the potency of S-flurbiprofen hydrazide hydrazones

  15. Efficacy and Tolerability of a Three-Step Acne System Containing a Solubilized Benzoyl Peroxide Lotion versus a Benzoyl Peroxide/Clindamycin Combination Product: An Investigator-Blind, Randomized, Parallel-Group Study

    OpenAIRE

    Green, Lawrence J.; Del Rosso, James Q.

    2008-01-01

    A brand three-step acne treatment system containing a solubilized 5% benzoyl lotion and a designated cleanser and moisturizer was compared with a brand benzoyl peroxide 5%/clindamycin 1% gel in subjects with acne vulgaris. The single-center, four-week study was investigator-blinded and randomized. The three-step acne treatment system proved to be comparable in efficacy and tolerability.

  16. SYNTHESIS OF POLYSTYRENE-BLOCK-POLYCAPROLACTAM WITH 1,1-BIS-(1'-NAPHTHYL) ETHYLENE AS A -DEACTIVATING AGENT

    Institute of Scientific and Technical Information of China (English)

    JIANG Rishan; QUIRK, Roderic P.

    1993-01-01

    The insertion of 1,1-bis (1'-naphthyl) ethylene monomer unit into the active polystyrene chain end greatly decreased the reactivity of the active chain end to the carbonyl group, and allowed the polymeric chain end to react only with the double bond in N-methacryloyl caprolactam, resulting in N-acylcaprolactam functionalized polystyrene in 100% conversion. New diblock copolymer of polystyrene with polycaprolactam was synthesized by direct reaction of the functionalized polymer with caprolactam without adding additional alkali metal or their caprolactam salts.

  17. Profile of clindamycin phosphate 1.2%/benzoyl peroxide 3.75% aqueous gel for the treatment of acne vulgaris

    Directory of Open Access Journals (Sweden)

    Nguyen TA

    2015-10-01

    Full Text Available Tuyet A Nguyen,1,2 Lawrence F Eichenfield1,31Division of Pediatric and Adolescent Dermatology, Rady Children's Hospital, San Diego, CA, 2Department of Medicine, Albert Einstein College of Medicine, Bronx, NY, 3Department of Dermatology, University of California, San Diego, La Jolla, CA, USA Abstract: Acne vulgaris is a common and chronic skin disease, and is a frequent source of morbidity for affected patients. Treatment of acne vulgaris is often difficult due to the multifactorial nature of this disease. Combination therapy, such as that containing clindamycin and benzoyl peroxide, has become the standard of care. Several fixed formulations of clindamycin 1% and benzoyl peroxide of varying concentrations are available and have been used with considerable success. The major limitation is irritation and dryness from higher concentrations of benzoyl peroxide, and a combination providing optimal efficacy and tolerability has yet to be determined. Recently, a clindamycin and benzoyl peroxide 3.75% fixed combination formulation was developed. Studies have suggested that this formulation may be a safe and effective treatment regimen for patients with acne vulgaris. Here, we provide a brief review of acne pathogenesis, benzoyl peroxide and clindamycin, and profile a new Clindamycin-BP 3.75% fixed combination gel for the treatment of moderate-to-severe acne vulgaris. Keywords: acne vulgaris, benzoyl peroxide, clindamycin

  18. Synthesis and characterization of bio-based polyurethane from benzoylated cashewnut husk tannins

    Indian Academy of Sciences (India)

    A J Sunija; S Siva Ilango; K P Vinod Kumar

    2014-05-01

    Benzoylated tannin prepared by benzoylation of cashewnut husk tannin, was treated with hexame-thylenediisocyanate in the presence of 1,4-butanediol as an extender to prepare thermosetting polyurethane. The sample was characterized using FT–IR and 13C NMR spectra. Thermal, morphological, physico-chemical and electrical properties were also investigated. Polyurethane obtained was sensitive to moisture but had very good solvent resistance. Results show that g of the sample is 260 °C and thermal decomposition begins at 280 °C. The dielectric constant varies randomly with temperature. The conductivity of the sample was found to increase with increase in temperature but shows random variation at 90 and 150 °C

  19. Benzoylation of anisole catalyzed by Ga/SBA-15 supported on carbon nanofibers composite

    OpenAIRE

    EL BERRICHI, F. Z.; Pham-Huu, C.; CHERIF, L.; Louis, B; M. J.; Ledoux

    2011-01-01

    Carbon nanofiber composite (C-NFC) shows several advantages compared to the conventional supports which are usually employed in catalysis such as alumina, silica or activated charcoal. In this present work we have developed a new hybrid catalyst consisting of SBA-15 supported on C-NFC for the benzoylation reaction. The structured materials allow an important improvement of the reaction hydrodynamics and favor the mass transfer between the active phase and the reactants, especially in the liqu...

  20. Synthesis and antiproliferative activity of novel 2-aryl-4-benzoyl-imidazole derivatives targeting tubulin polymerization

    OpenAIRE

    Chen, Jianjun; Li, Chien-Ming; Wang, Jin; Ahn, Sunjoo; Wang, Zhao; Lu, Yan; Dalton, James T.; Miller, Duane D.; Li, Wei

    2011-01-01

    We previously reported the discovery of 2-aryl-4-benzoyl-imidazoles (ABI-I) as potent antiproliferative agents for melanoma. To further understand the structural requirements for the potency of ABI analogs, gain insight in the structure-activity relationships (SAR), and investigate metabolic stability for these compounds, we report extensive SAR studies on the ABI-I scaffold. Compared with the previous set of ABI-I analogs, the newly synthesized ABI-II analogs have lower potency in general, b...

  1. Chromatographic determination of metal ions after complexation with bis(quaternary ammonium hydrazones) of 2,6-diacetylpyridine

    International Nuclear Information System (INIS)

    Two new bis hydrazones of 2,6-diacetylpyridine were prepared and characterized. Both of these contain a quaternary ammonium group that greatly enhances the water solubility of the reagent and its metal-ion complexes. When the solid reagent was dissolved in water, an equilibrium was attained in which three geometric forms coexist. A rate constant was determined for this equilibrium. Several metal ions were determined quantitatively and selectively by complexation with one of the bis hydrazones and chromatographic separation of the metal ion complexes. Interferences due to the presence of other ions in solution were investigated

  2. Synthesis and Crystal Structure of Binuclear Ytterbium Complex with Isonicotinoyl Hydrazone

    Institute of Scientific and Technical Information of China (English)

    卜显和; 鹿守亮; 陈巍; 张若桦

    2001-01-01

    The ytterbium complex of isonicotinoyl hydrazone was synthesized and the structure was determined by X-ray diffraction analysis. The crystal and molecular structure of the title complex [Yb2(L)3](OH)3 shows that the complex has two identical nine-coordinated ytterbium ions with each surrounded by N3O6 donor set. Two ytterbium ions are bridged by three phenolate oxygen atoms. The geometry around each ytterbium ions can be considered as a three-capped trigonal prism.

  3. Iron(III)-Mediated Radical Nitration of Bisarylsulfonyl Hydrazones: Synthesis of Bisarylnitromethyl Sulfones.

    Science.gov (United States)

    Sar, Dinabandhu; Bag, Raghunath; Bhattacharjee, Debajyoti; Deka, Ramesh Chandra; Punniyamurthy, Tharmalingam

    2015-07-01

    Iron(III)-mediated radical nitration of bisarylsulfonyl hydrazones is described. In this protocol, the nontoxic and inexpensive Fe(NO3)3·9H2O plays a dual role as catalyst as well as nitro source. The mild conditions, broad substrate scope, and the functional group compatibility are the significant features. The reaction pathway has been demonstrated using DFT calculations, and the products can be subsequently converted into oximes using SnCl2·2H2O in high yields. PMID:26036359

  4. Persistent Enhanced Conductivity Induced by Light Irradiation in Hydrazone-Polycarbonate Dispersions

    Science.gov (United States)

    Hirao, Akiko; Nishizawa, Hideyuki; Hosoya, Masahiro

    1994-04-01

    Photoinduced spins with extended lifetime have been observed in hydrazone-polycarbonate dispersions. The presence of the spins changed the electrical characteristics of the dispersions. Measurements of electrical current associated with thermal equilibration after photoexcitation in dispersions of diethylamino-benzaldehyde diphenylhydrazone (DEH) in polycarbonate have been carried out. Sandwiched layers of the dispersions were excited with absorbed light. After withdrawal of the light, a voltage was applied and the current was measured. Experimental data provide evidence that photoinduced spins are derived from trapped carriers.

  5. Synthesis of Benzophenone Hydrazone Analogs and their DPPH Radical Scavenging and Urease Inhibitory Activates

    International Nuclear Information System (INIS)

    Benzophenone hydrazone analogs 1-25 were synthesized and evaluated for antioxidant (DPPH radical scavenging), and urease inhibitory activities. Out of twenty-five analogs, compounds 8, 23, and 1 showed potent free radical scavenging activities with IC50 values 19.45 ± 1.25, 21.72 ± 1.49, and 26.0 ± 0.52 μM, respectively, while compound 8 (IC50 = 36.36 ± 0.94 μ M), and 15 (IC50 = 55.5 ± 0.69 μ M), showed good to moderate urease inhibitory potential. (author)

  6. Kinetics and Mechanistic Study of Permanganate Oxidation of Fluorenone Hydrazone in Alkaline Medium

    OpenAIRE

    Fawzy, Ahmed; Saleh A. Ahmed; Althagafi, Ismail I.; Morad, Moataz H.; Khairou, Khalid S

    2016-01-01

    The oxidation kinetics of fluorenone hydrazone (FH) using potassium permanganate in alkaline medium were measured at a constant ionic strength of 0.1 mol dm−3 and at 25°C using UV/VIS spectrophotometer. A first-order kinetics has been monitored in the reaction of FH with respect to [permanganate]. Less-than-unit order dependence of the reaction on [FH] and [OH−] was revealed. No pronounced effect on the reaction rate by increasing ionic strength was recorded. Intervention of free radicals was...

  7. Electrooxidation of carbo/thiocarbohydrazide and their hydrazone derivatives at a glassy carbon electrode

    Indian Academy of Sciences (India)

    G P Mamatha; B S Sherigara; K M Mahadevan

    2007-05-01

    Electrochemical oxidation of thio/carbohydrazide and their hydrazone derivatives Benzaldehyde thiocarbohydrazone [BTCH] diacetylene thiocarbohydrazone [DATCH] have been studied in Britton Robinson buffer in aqueous and nonaqueous media at a glassy carbon electrode. The effects of pH, sweep rate, concentration, temperature and surfactants have been studied. The complex bis (carbo/thiocabohydrazide) Zn(II) chloride was also subjected to voltammetric analysis in order to understand the reactivity both in free and metal bound states. The reaction conditions were optimized for the determination of above compounds in micrograms quantities by differential pulse voltammetry, analytical utility of this investigation is also highlighted.

  8. Use of Hydrazone Derivates as Inhibitors for the Corrosion of Nickel in Hydrochloric Acid Solution

    Directory of Open Access Journals (Sweden)

    A.S. Fouda, H. A. Mostafa, S. E. Ghazy and S. A. El- Farah

    2007-02-01

    Full Text Available The influence of hydrazone derivatives on the corrosion of nickel in 2 mol L-1 hydrochloric acid solution has been studied using weight loss and galvanostatic polarization techniques. In general, at constant acid concentration, the inhibition efficiency increases with increasing the inhibitor concentration and decreases with increasing temperature. Polarization studies indicate that the compounds act as mixed- type inhibitors. The addition of iodide ions enhances the inhibition efficiency to a considerable extent .The effect of temperature on corrosion inhibition has been studied and activation energy has been calculated. Some thermodynamic parameters are calculated and discussed.

  9. Efficacy and safety of topical nadifloxacin and benzoyl peroxide versus clindamycin and benzoyl peroxide in acne vulgaris: A randomized controlled trial

    Directory of Open Access Journals (Sweden)

    S Choudhury

    2011-01-01

    Full Text Available Background : Topical therapy with comedolytics and antibiotics are often advocated for mild and moderate severity acne vulgaris. Nadifloxacin, a new fluoroquinolone with anti-Propionibacterium acnes activity and additional anti-inflammatory activity, is approved for use in acne. This randomized controlled assessor blind trial compared the clinical effectiveness and safety of eight weeks therapy of nadifloxacin 1% versus clindamycin 1% as add-on therapy to benzoyl peroxide (2.5% in mild to moderate grade acne. Materials and Methods : The efficacy parameters were changes in the total, inflammatory and non-inflammatory lesion counts, Investigator Global Assessment (IGA, and Cardiff Acne Disability Index (CADI scales from baseline to study end (eight weeks. All treatment emergent dermatological adverse events were evaluated for safety assessment. Results : Out of 84 randomized subjects (43-nadifloxacin arm and (41-clindamycin 42 in nadifloxacin group, 37 in clindamycin group completed the study. Reduction from baseline of total, inflammatory and non-inflammatory lesion counts were highly significant in both the groups (P<0.0001, but between group differences were not significant. Significant improvement in CADI and IGA scales were noted in both groups. Between-group comparison showed no significant differences. The safety and tolerability profile of both regimens were good and statistically comparable. Conclusions: Topical nadifloxacin, a new fluoroquinolone is effective, tolerable, and safe for mild o moderate facial acne. Its clinical effectiveness is comparable to clindamycin when used as add-on therapy to benzoyl peroxide.

  10. Analysis of benzoyl-peroxide and formaldehyde as dental allergens by FT-SPR method

    International Nuclear Information System (INIS)

    In parallel with the appearance of new dental materials the number of induced allergic diseases increases. Based on this fact more sensitive detection of allergens is major importance. The Fourier-Transform Surface Plasmon Resonance (FT-SPR) is a sensitive, broadly applicable real-time method for analysing thin layers of materials on gold surfaces. FT-SPR measurement is performed at a fixed angel of incident light, and reflectivity is measured over a range of wavelength in the near infrared. In our study the formaldehyde and benzoyl-peroxide were examined as members of the most common dental allergens by FT-SPR spectroscopy. The aim of this work was the investigation of the suitability of this method for the direct detection of these materials. Different concentrations of formaldehyde and benzoyl-peroxide solutions were measured from this purpose. The individual spectra were measured for all of the solutions, and calibration curves were calculated for the materials for the possibility of the determination of an unknown concentration. In addition, series measurements were performed whereby the association and dissociation properties of formaldehyde or benzoyl-peroxide were described. The results of the experiments proved that the method capable to measure directly these materials and can provide appropriate calibration curves for determination of unknown concentrations

  11. PREPARATION, CHARACTERIZATION AND ADHESIVE PROPERTIES OF DI-AND TRI-HYDROXY BENZOYL CHITOSAN NANOPARTICLES

    Institute of Scientific and Technical Information of China (English)

    Mohamad Taghi Taghizadeh; Ali Bahadori

    2013-01-01

    Modified chitosans with 3,4-di-hydroxy benzoyl groups (CS-DHBA) and 3,4,5-tri-hydroxy benzoyl groups (CSTHBA) were synthesized and their nanoparticles were prepared via ionic crosslinking by tripolyphosphate (TPP).The chemical structure and degree of substitution (DS) of di-and tri-hydroxy benzoyl chitosans are determined by FTIR and 1HNMR spectroscopy.The morphology of particles,size distribution and zeta potential of nanoparticles were studied using transmission electron microscopy (TEM) and dynamic light scattering (DLS),respectively.The mean diameters of particles of CS-DHBA and CS-THBA nanoparticles were 144 nm and 112 nm,respectively.It was found that the particles size decreased slightly with decreasing the degree of substitution and increasing degree of deacetylation (DD),due to increasing of ionic crosslinking of ammonium ions and polyanions of tripolyphosphate.The TEM photographs of CS-DHBA show that these particles are spherical in shape,but the particles of CS-THBA show some aggregation.In addition,the solubility and the mechanical properties of the prepared modified chitosans and their nanoparticles were evaluated for bio-adhesive and biomedical application.The results of solubility tests indicated that,the CS-DHBA and CS-THBA have higher solubility at pH > 7 comparing to CS.Also the CS-DHBA,CS-THBA and their nanoparticles showed a significant adhesive capacity and enhanced tensile strength and tensile modulus.

  12. The synthesis and unusual luminescence behavior of 1,1-dimethyl-2,5-di(2-naphthyl)-3,4-diphenylsilole

    International Nuclear Information System (INIS)

    The synthesis and spectroscopic characteristics, including quantum yield and luminescence lifetime, of 1,1-dimethyl-2,5-di(2-naphthyl)-3,4-diphenylsilole are described. Unlike most aryl substituted siloles, the compound displays very efficient luminescence in solution, but does not exhibit aggregation-induced emission. In addition, the solution-phase emission intensity demonstrates an unusual time dependence. - Highlights: ► Novel naphthyl-substituted silole with large luminescence quantum yield. ► The silole exhibits aggregation-caused quenching. ► The compound displays a time-dependent emission intensity. ► Luminescence lifetimes are reported.

  13. Vanadium Complexes with Hydrazone or Thiosemicarbazone Ligands as Potential Anti-Mycobacterium tuberculosis Agents.

    Science.gov (United States)

    de Souza, Paula C; Maia, Pedro I S; de Barros, Heloisa B; Leite, Clarice Q F; Deflon, Victor M; Pavan, Fernando R

    2015-01-01

    Tuberculosis (TB) is an infectious disease caused mainly by Mycobacterium tuberculosis (MTB) and still an important public health problem worldwide. Some factors like the emergence of multidrug resistant (MDR) and extensively drug-resistant (XDR) strains make urgent the research of new active compounds. Searching for new inorganic compounds against TB, three new dioxovanadium(V) complexes were obtained upon reaction of [VO(acac)2] with hydrazone and thiosemicarbazone ligands derived from di-2-pyridyl ketone. Spectroscopic studies and X-ray crystallography revealed asymmetrically oxo bridged binuclear complexes of the type [{VO(L(1,2))}2(μ-O)2], involving the hydrazone ligands, while a mononuclear square pyramidal complex of the type [VO2(L(3))] was formed with the thiosemicarbazone ligand. The compounds were tested against M. tuberculosis and three of them, with MICs values between 2.00 and 3.76 μM were considered promising for TB treatment. Such MIC values are comparable or better than those found for some drugs currently used in TB treatment. PMID:24433444

  14. Synthesis, spectral characterization, DNA interaction, radical scavenging and cytotoxicity studies of ruthenium(II) hydrazone complexes.

    Science.gov (United States)

    Mohanraj, Maruthachalam; Ayyannan, Ganesan; Raja, Gunasekaran; Jayabalakrishnan, Chinnasamy

    2016-05-01

    Three new ruthenium(II) complexes with hydrazone ligands, furan-2-carboxylic acid (2,4-dihydroxy-benzylidene)-hydrazide (HL(1)), furan-2-carboxylic acid [4-(ethyl-propyl-amino)-2-hydroxy-benzylidene]-hydrazide (HL(2)) and furan-2-carboxylic acid (3-ethoxy-2-hydroxy-benzylidene)-hydrazide (HL(3)) were synthesized and characterized by various spectro-analytical techniques. The hydrazone ligands act as a tridendate ligand with ONO as the donor sites and are preferably found in the enol form in all the complexes. The molecular structure of the ligands was determined by single crystal X-ray diffraction technique. The interaction of the ligands and the complexes with CT-DNA were evaluated by an absorption titration method which revealed that the compounds interact with CT-DNA through intercalation. Gel electrophoresis assay demonstrated the ability of the complexes to cleave the calf thymus DNA hydrolytically. Antioxidant studies showed that the ruthenium(II) complexes have a strong radical-scavenging properties. Further, the cytotoxic effect of the compounds examined on cancerous cell lines showed that the complexes exhibited substantial anticancer activity. PMID:26974577

  15. Synthesis and Conformational Assignment of N-(E-Stilbenyloxymethylenecarbonyl-Substituted Hydrazones of Acetone and o-(m- and p- Chloro- (nitro- benzaldehydes by Means of and NMR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Przemysław Patorski

    2013-01-01

    Full Text Available Eighteen new N-(E-stilbenyloxyalkylcarbonyl-substituted hydrazones of ortho- (meta- and para- chloro- (nitro- benzaldehydes 1–18 and two analogous hydrazones of acetone 19-20 were prepared. The stereochemical behavior of 1–18 in dimethyl-d6 sulfoxide solution has been studied by NMR and NMR techniques, using spectral data of 19 and 20 as supporting material. The E-geometrical isomers and cis-/trans-amide conformers have been found for these hydrazones. Energy barriers of isomers are reported.

  16. Organic light-emitting diodes based on 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit as the deep-blue emitting layer

    Energy Technology Data Exchange (ETDEWEB)

    Song, Ji Young; Lee, Seul Bee [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Lee, Seok Jae [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@wow.hongik.ac.kr [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2015-02-27

    A series of 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit, which prevented molecular aggregation and self-quenching effect, was designed and synthesized. By using various bridges between the 9-(2-naphthyl)anthracene group and the triphenylsilane unit, five deep-blue emitters were obtained and applied as non-doped emitting materials in organic light-emitting diodes (OLEDs) with a device structure of indium–tin-oxide (ITO) (180 nm)/4,4-bis(N-(1-naphthyl)-N-phenylamino)biphenyl (NPB) (50 nm)/emitting materials (30 nm)/4,7-diphenyl-1,10-phenanthroline (Bphen) (30 nm)/lithium quinolate (Liq) (2 nm)/Aluminium (100 nm). All devices showed blue emissions and their electroluminescence efficiencies are sensitive to the structural changes of the emitting materials. In particular, a device using 9-(2-naphthalenyl)-10-[6-(triphenylsilyl)-2-naphthalenyl]-anthracene (4) exhibited high luminous, power and quantum efficiencies of 2.28 cd/A, 1.42 lm/W and 2.40% at 20 mA/cm{sup 2}, respectively, and this device showed the deep blue emission with the CIE coordinates of (0.16, 0.10) at 6.0 V. - Highlights: • We synthesized 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit. • We study the conjugation-length effect on the electroluminescence properties. • The bulky triphenylsilane-anthracene derivatives show resistance to self-aggregation.

  17. Organic light-emitting diodes based on 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit as the deep-blue emitting layer

    International Nuclear Information System (INIS)

    A series of 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit, which prevented molecular aggregation and self-quenching effect, was designed and synthesized. By using various bridges between the 9-(2-naphthyl)anthracene group and the triphenylsilane unit, five deep-blue emitters were obtained and applied as non-doped emitting materials in organic light-emitting diodes (OLEDs) with a device structure of indium–tin-oxide (ITO) (180 nm)/4,4-bis(N-(1-naphthyl)-N-phenylamino)biphenyl (NPB) (50 nm)/emitting materials (30 nm)/4,7-diphenyl-1,10-phenanthroline (Bphen) (30 nm)/lithium quinolate (Liq) (2 nm)/Aluminium (100 nm). All devices showed blue emissions and their electroluminescence efficiencies are sensitive to the structural changes of the emitting materials. In particular, a device using 9-(2-naphthalenyl)-10-[6-(triphenylsilyl)-2-naphthalenyl]-anthracene (4) exhibited high luminous, power and quantum efficiencies of 2.28 cd/A, 1.42 lm/W and 2.40% at 20 mA/cm2, respectively, and this device showed the deep blue emission with the CIE coordinates of (0.16, 0.10) at 6.0 V. - Highlights: • We synthesized 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit. • We study the conjugation-length effect on the electroluminescence properties. • The bulky triphenylsilane-anthracene derivatives show resistance to self-aggregation

  18. Structure-activity relationships of novel salicylaldehyde isonicotinoyl hydrazone (SIH analogs: iron chelation, anti-oxidant and cytotoxic properties.

    Directory of Open Access Journals (Sweden)

    Eliška Potůčková

    Full Text Available Salicylaldehyde isonicotinoyl hydrazone (SIH is a lipophilic, tridentate iron chelator with marked anti-oxidant and modest cytotoxic activity against neoplastic cells. However, it has poor stability in an aqueous environment due to the rapid hydrolysis of its hydrazone bond. In this study, we synthesized a series of new SIH analogs (based on previously described aromatic ketones with improved hydrolytic stability. Their structure-activity relationships were assessed with respect to their stability in plasma, iron chelation efficacy, redox effects and cytotoxic activity against MCF-7 breast adenocarcinoma cells. Furthermore, studies assessed the cytotoxicity of these chelators and their ability to afford protection against hydrogen peroxide-induced oxidative injury in H9c2 cardiomyoblasts. The ligands with a reduced hydrazone bond, or the presence of bulky alkyl substituents near the hydrazone bond, showed severely limited biological activity. The introduction of a bromine substituent increased ligand-induced cytotoxicity to both cancer cells and H9c2 cardiomyoblasts. A similar effect was observed when the phenolic ring was exchanged with pyridine (i.e., changing the ligating site from O, N, O to N, N, O, which led to pro-oxidative effects. In contrast, compounds with long, flexible alkyl chains adjacent to the hydrazone bond exhibited specific cytotoxic effects against MCF-7 breast adenocarcinoma cells and low toxicity against H9c2 cardiomyoblasts. Hence, this study highlights important structure-activity relationships and provides insight into the further development of aroylhydrazone iron chelators with more potent and selective anti-neoplastic effects.

  19. Coordination Structure Conversion of Hydrazone-Palladium(II) Complexes in the Solid State and in Solution.

    Science.gov (United States)

    Kitamura, Fumi; Sawaguchi, Kana; Mori, Asami; Takagi, Shoji; Suzuki, Takayoshi; Kobayashi, Atsushi; Kato, Masako; Nakajima, Kiyohiko

    2015-09-01

    We prepared hydrazone-palladium(II) complexes of [PdCl2(HL(n))] and [PdCl(L(n))] (n = 1-3) by the reaction of [PdCl2(cod)] or [PdCl2(PhCN)2] and the hydrazone ligands of HL(n) {N'-(pyridin-2-ylmethylene)picolinohydrazide (HL(1)), N'-[1-(pyridin-2-yl)ethylidene]picolinohydrazide (HL(2)), and N'-[(6-methylpyridin-2-yl)methylene]picolinohydrazide (HL(3))}. The structures of the complexes were determined by X-ray analysis. The hydrazone ligands had κN(py1),κN(imine) and κN(amidate),κN(py2) bidentate coordination modes in [PdCl2(HL(n))] (1, n = 1; 2, n = 2) and in [PdCl2(HL(3))] (3), respectively. In contrast, tridentate coordination modes of κN(py1),κN(imine),κN(py2) and κN(py1),κN(amidate),κN(py2) were observed in [PdCl(L(n))] (4, n = 1; 5, n = 2) and in [PdCl(L(n))] (6, n = 1; 7, n = 2; 8, n = 3). Thermal conversion of complexes 1-3 to complexes 6-8 proceeded in acetonitrile. Complexes 4 and 5 were obtained from complexes 1 and 2, respectively, in a basic acetonitrile solution under dark conditions. Complex 4 reverted immediately to complex 1 in an acidic acetonitrile solution that included hydrochloric acid. However, under room light, in the basic acetonitrile solution that included trimethylamine, complex 4 converted photochemically to complex 6. The thermochromic or vapochromic structure conversion of these complexes also occurred in the solid state. On heating at 180 °C, the color of the crystals of complexes 1, 2, and 3 changed from yellow to orange in the solid state. (1)H NMR and/or UV-vis absorption spectroscopy confirmed that the orange complexes 6-8 were produced. The reddish-orange crystals of complexes 4 and 5 were exposed to hydrogen chloride vapor to yield the yellow products of complexes 1 and 2, respectively. PMID:26305775

  20. Biosynthesis of benzoylformic acid from benzoyl cyanide with a new bacterial isolate of Brevibacterium sp. CCZU12-1.

    Science.gov (United States)

    He, Yu-Cai; Pan, Xue-He; Xu, Xiao-Feng; Wang, Li-Qun

    2014-03-01

    Brevibacterium sp. CCZU12-1 with high nitrilase activity could effectively hydrolyze benzoyl cyanide into benzoylformic acid. After the culture optimization, the preferred carbon sources, nitrogen sources, and inducer were glucose (10 g/L), a composite of peptone (10 g/L) plus yeast extract (2.5 g/L), and ε-caprolactam (2.0 mM), respectively. After the reaction optimization, the optimum reaction temperature, reaction pH, organic cosolvent, and metal ion were 30 °C, 7.0, ethanol (2%, v/v), and Ca(2+) (0.1 mM), respectively. At biotransformation of 120-mM benzoyl cyanide for 24 h, the yield of benzoylformic acid reached 91.8%. Moreover, the microbial nitrilase from Brevibacterium sp. CCZU12-1 could hydrolyze various nitriles, and it significantly exhibited high nitrilase activity against benzoyl cyanide, 3-cyanopyridine, and α-cyclohexyl-mandelonitrile. PMID:24504691

  1. 2-Benzoyl-4-chloro­aniline thio­semi­carbazone

    OpenAIRE

    Katlen C. T. Bandeira; Leandro Bresolin; Lehmann, Ueslei Z.; Priscilla J. Zambiazi; Adriano Bof de Oliveira

    2014-01-01

    In the title compound, C14H13ClN4S, obtained from a reaction of 2-benzoyl-4-chloro­aniline with thio­semicarbazide in ethanol, the dihedral angle between the aromatic rings is 81.31 (13)°. In the crystal, the mol­ecules are linked by three N—H⋯S hydrogen bonds, forming centrosymmetric rings with set-graph motif R 2 2(8) and R 2 2(18), and resulting in the formation of a two-dimensional network lying parallel to (010).

  2. Solvent extraction of lanthanide ions with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP)

    International Nuclear Information System (INIS)

    The solvent extraction of Er(3), Yb(3) and Lu(3) by 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5(HPMBP or HL) in carbon tetrachloride has been studied as a function of the pH of the aqueous phase and the concentration of the extractant in the organic phase. The equation for the extraction reaction has been suggested as: Ln3++3HL(0) rightleftdblarrow LnL3(0)+3H+(Ln3+ = Er, Yb, Lu). The extraction equilibrium constants (Kex) and two-phase stability constants (β3x) for the LnL3 complexes have been evaluated. (Author)

  3. Auto oxidation of plutonium with 3-phenyl-4-benzoyl-5-isoxazolone as an extractant

    International Nuclear Information System (INIS)

    Extraction of Pu (III) using 3-phenyl-4-benzoyl-5-isoxazolone (HPBI) was investigated in the presence of several reducing agents. It was observed that Pu (IV) was the dominating species extracted even though the aqueous phase comprised exclusively of Pu (III) initially. While aqueous reducing agents such as hydrazinium nitrate, hydroxyl ammonium nitrate, di-ethyl hydroxyl amine had no effect in suppressing the oxidation of Pu (III); organophilic t-butyl hydroquinone was found to be an effective holding reductant. The observed rate constants for the oxidation reaction were calculated and were found to be independent on the hydrogen ion concentration. (author)

  4. Photocarcinogenesis and toxicity of benzoyl peroxide in hairless mice after simulated solar radiation

    DEFF Research Database (Denmark)

    Lerche, Catharina M; Philipsen, Peter A; Poulsen, Thomas;

    2010-01-01

    Topical benzoyl peroxide (BPO) gel has long been used to treat acne vulgaris and has recently been combined with clindamycin (BPO-clin). No skin malignancies have been reported after clinical use of BPO, but there has been concern about the possible carcinogenicity of BPO alone and in combination...... with UV radiation. BPO can promote skin tumorigenesis in a mouse skin chemical carcinogenesis model. As acne vulgaris is frequently localized on sun-exposed areas, we investigated whether BPO or BPO-clin accelerates photocarcinogenesis in combination with simulated solar radiation (SSR) in 12 groups of...

  5. Benzoyl peroxide increases UVA-induced plasma membrane damage and lipid oxidation in murine leukemia L1210 cells.

    Science.gov (United States)

    Ibbotson, S H; Lambert, C R; Moran, M N; Lynch, M C; Kochevar, I E

    1998-01-01

    Ultraviolet A radiation induces oxidative stress and cell damage. The purpose of this investigation was to examine whether ultraviolet A-induced cell injury was amplified by the presence of a non-ultraviolet A absorbing molecule capable of generating free radicals. Benzoyl peroxide was used as a lipid soluble potential radical-generating agent. Plasma membrane permeability assessed by trypan blue uptake was used to measure cell damage in murine leukemia L1210 cells. Cells were irradiated with a pulsed Nd/YAG laser at 355 nm using 0-160 J per cm2. The ratio of the fluence-response slope in the presence of 40 microM benzoyl peroxide to that of irradiated controls was 4.3 +/- 2.6. Benzoyl peroxide alone or benzoyl peroxide added after irradiation did not cause increased trypan blue uptake. The ratio of the fluence-response slopes in the presence of 40 microM benzoyl peroxide to that of irradiated controls was 4.7 +/- 1.4 when cells were irradiated (0-43 J per cm2) with a xenon lamp, filtered to remove wavelengths butylated hydroxytoluene, vitamin E, and trolox, a water-soluble vitamin E derivative. Lipid oxidation, assessed as thiobarbituric acid reactive substances, was significantly increased in samples irradiated with ultraviolet A in the presence of benzoyl peroxide at fluences >34 J per cm2. The increased trypan blue uptake and thiobarbituric acid reactive substances were inhibited by butylated hydroxytoluene. These results suggest that agents not absorbing ultraviolet A radiation may enhance ultraviolet A-initiated oxidative stress in cells. PMID:9424093

  6. Dynamic Combinatorial Chemistry and Organocatalysis with Thiosemicarbazones and Organocatalysts for Hydrazone and Oxime Bioconjugations

    DEFF Research Database (Denmark)

    Larsen, Dennis

    The first part of this thesis describes the use of thiosemicarbazones for dynamic combinatorial chemistry. Building blocks incorporating thiosemicarbazides and acetalprotected aldehydes were synthesised and conditions where these building blocks formed dynamic combinatorial libraries under...... of this thesis describes the development of new bifunctional organocatalysts for the formation of hydrazones and oximes at neutral pH. New effective variants of the previously known anthranilic acid-based catalysts were discovered, and via a virtual breakdown of the structure of already identified...... catalysts, two new types of catalysts were discovered: The 2-aminophenols and the 2-(aminomethyl)benzimidazoles. With aldehyde substrates none of the newly discovered catalysts were as effective as a previously discovered benzenephosphonic acid, but with aromatic ketones, an otherwise challenging class of...

  7. Verification of the dispersive charge transport in a hydrazone:polycarbonate molecularly doped polymer

    International Nuclear Information System (INIS)

    We report results of specially planned experiments intended to verify the dispersive character of the charge carrier transport in polycarbonate molecularly doped with hydrazone at 30 wt% loading, using for this purpose samples specifically featuring a well-defined plateau on a linear-linear plot. For this purpose we propose a new variant of the time-of-flight technique which allows easy changing of the generation zone width from about 0.5 μm (surface excitation) through intermediate values to full sample thickness (bulk excitation). To achieve this, we use electron pulses of 3-50 keV energy rather than traditional light pulses provided by lasers. Experimental results corroborated by numerical calculations uniquely prove that carrier transport in this molecularly doped polymer is dispersive, with the dispersion parameter equal to 0.75. Nevertheless, the mobility field dependence follows the famous Poole-Frenkel law.

  8. Synthesis and anticandidal evaluation of new benzothiazole derivatives with hydrazone moiety.

    Science.gov (United States)

    Yurttaş, Leyla; Kaplancıklı, Zafer Asım; Göger, Gamze; Demirci, Fatih

    2016-10-01

    In this study, we have performed the synthesis of new N'-(arylidene)-4-[(benzothiazol-2-yl)thio]butanoylhydrazide derivatives (3a-s) bearing azole moiety and hydrazone group in a lipophilic structural framework. The target compounds were prepared by a three step synthetic procedure starting from 2-mercaptobenzothiazole. The structures of the target compounds were elucidated by IR, (1)H NMR, (13)C NMR spectra and elemental analysis. The antifungal activity of the obtained compounds has been determined against a number of clinic and fluconazole-resistant Candida strains by using microdilution method. Compounds (3a-3s) exhibited anticandidal activity in different ratios varying between the range of MIC: 50 and 200 µg/mL. PMID:26247354

  9. Derivative spectrophotometric determination of uranium (VI using diacetyl monoxime isonicotinoyl hydrazone (DMIH

    Directory of Open Access Journals (Sweden)

    ChandraSekhar Reddy Gadikota

    2011-08-01

    Full Text Available Uranium (VI forms a yellow coloured water soluble complex with diacetyl monoxime isonicotinoyl hydrazone (DMIH reagent in acidic buffer of pH 3.25 with ?max at 364 nm. The molar absorptivity and sandell’s sensitivity are 1.63 X 10 4 L.mol -1.cm-1 and 0.00307692 µg/cm 2, respectively. The Beer’s law validity range is 1.19–14.28 µg/mL. Uranium (VI forms (M:L 1:1 complex with DMIH and stability constant of the complex is 4.928 X 106 .The derivative spectrophotometric determination of U (VI was carried out by measuring peak height method. The developed derivative spectrophotometric method was employed for the determination of uranium (VI in rock and synthetic samples. The effect of various diverse ions was also studied.

  10. Synthesis, activity evaluation, and docking analysis of barbituric acid aryl hydrazone derivatives as RSK2 inhibitors.

    Science.gov (United States)

    Xue, Mengzhu; Xu, Minghao; Lu, Weiqiang; Huang, Jin; Li, Honglin; Xu, Yufang; Liu, Xiaofeng; Zhao, Zhenjiang

    2013-08-01

    The 90 kDa ribosomal S6 kinases (RSKs), especially RSK2, have attracted attention for the development of new anticancer agents. Through structural optimization of the hit compound 1 from our previous study, a series of barbituric acid aryl hydrazone analogues were designed and synthesized as potential RSK2 inhibitors. The most potent one, compound 9, showed a higher activity against RSK2 with an IC50 value of 1.95 μM. To analyze and elucidate their structure-activity relationship, the homology model of RSK2 N-terminal kinase domain was built and molecular docking simulations were performed, which provide helpful clues to design new inhibitors with desired activities. PMID:22545939

  11. Design, synthesis, and insecticidal activities of new N-benzoyl-N'-phenyl-N'-sulfenylureas.

    Science.gov (United States)

    Sun, Ranfeng; Zhang, Yonglin; Chen, Li; Li, Yongqiang; Li, Qingshan; Song, Haibin; Huang, Runqiu; Bi, Fuchun; Wang, Qingmin

    2009-05-13

    A series of new N'-alkylaminothio, N'-arylaminothio (or dithio), and N',N'-thio (or dithio) derivatives of N-benzoyl-N'-phenylureas were designed and synthesized as insect-growth regulators with sulfur dichloride or disulfur dichloride as the original reactant. The new compounds were identified by (1)H nuclear magnetic resonancee (NMR) spectroscopy, elemental analysis [or high-resolution mass spectrometry (HRMS)], and single-crystal X-ray diffraction analysis. The X-ray results demonstrated that there exist N-S-N or N-S-S-N bonds in these new compounds. In comparison to the parent N-benzoyl-N'-phenylureas, these derivatives displayed better solubility. The insecticidal activities of the target compounds were evaluated. The results of bioassays showed that compounds 1-24 retained the larvicidal activities of the corresponding benzoylphenylureas (BPUs) and some compounds exhibited better larvicidal activities against oriental armyworm and mosquitoes than the parent BPUs. The larvicidal activities of the selected target compounds 1 and 24 against diamondback moth were better than that of the corresponding parent compounds E and triflumuron. PMID:19326865

  12. n-Benzoyl-n-phenylhydroxylamine impregnated Amberlite XAD-4 beads for selective removal of thorium

    International Nuclear Information System (INIS)

    Highlights: • XAD-4 was impregnated with a commonly used gravimetric agent n-benzoyl-n-phenylhydroxylamine. • Sorbent characterized by different techniques to understand the pore filling of XAD-4. • Sorption of Th was fast (30 min) and unaffected by initial solution pH. • Selectivity achieved by tuning the conditions of the mixture solution. - Abstract: n-Benzoyl-n-phenylhydroxylamine impregnated Amberlite XAD-4 beads were used for the removal of Th(IV) from a mixture of ions. The impregnated XAD was characterized using different techniques like weight and colour change, IR spectra, surface area and pore size measurements to confirm the presence of n-BPHA within the macroreticular resin structure. The experimental conditions were optimized to make the separation fast and selective. It was seen that the maximum sorption was achieved in the pH range of 3–7.5 and uptake was nearly complete within half an hour. The results obtained in the present study were subjected to extensive modelling in order to get a complete understanding of the sorption process. It is seen that the maximum uptake was calculated to be 500 mg/g and has very fast kinetics it was seen that the process is chemisorption. It was further deduced from the modelling that the overall sorption process was controlled dominantly by external mass transfer. Considering the simplicity this procedure, the present study has a possible application for the removal of thorium from different mixtures

  13. Characterization of a newly synthesized organic nonlinear optical crystal: benzoyl valine

    Science.gov (United States)

    Kumar, T. K.; Selvaraj, R. S.; Janarthanan, S.; Rajan, Y. C.; Selvakumar, S.; Pandi, S.; Selvakumar, M. S.; Anand, D. P.

    2010-05-01

    Herein the synthesis and the crystal growth of benzoyl valine (BV), an organic nonlinear optical (NLO) material for frequency conversion was grown by slow evaporation solution growth technique at room temperature has been reported. The compound was prepared by Stockman method of benzoylation. The solubility curve shows linear nature up to a temperature of 313 K. XRD study reveals that the crystal belongs to monoclinic system with P21 non-centrosymmetric space group. The fundamental vibrational frequency of various functional groups (400-4000 cm-1) in the crystal was determined from FTIR analysis. 1H and 13C NMR spectral studies reveal the presence of proton and carbon network in the grown crystalline sample. The optical behaviour of the crystal was ascertained by optical UV absorption spectral studies. The UV cut off region (λmax) lies around 200 nm and the crystal is absolutely transparent from 220-800 nm suggesting its application as NLO material. The thermal stability of the crystal was determined by thermogravimetric and differential thermal analyses. Laser damage threshold of BV was found to be 0.34 GW/cm2 and hence BV can be used in frequency doubler system. Photoconductivity study of BV revealed negative photoconductiviting nature of the sample. The microhardness studies confirm that BV has a moderate Vickers hardness number (VHN) value in comparison to the other organic NLO crystals.

  14. Design, synthesis, and anti-melanogenic effects of (E-2-benzoyl-3-(substituted phenylacrylonitriles

    Directory of Open Access Journals (Sweden)

    Yun HY

    2015-08-01

    Full Text Available Hwi Young Yun,1 Do Hyun Kim,1 Sujin Son,1 Sultan Ullah,1 Seong Jin Kim,1 Yeon-Jeong Kim,2 Jin-Wook Yoo,1 Yunjin Jung,1 Pusoon Chun,2 Hyung Ryong Moon1 1College of Pharmacy, Pusan National University, Busan, 2College of Pharmacy, Inje University, Gimhae, Republic of Korea Background: Tyrosinase is the most prominent target for inhibitors of hyperpigmentation because it plays a critical role in melaninogenesis. Although many tyrosinase inhibitors have been identified, from both natural and synthetic sources, there remains a considerable demand for novel tyrosinase inhibitors that are safer and more effective. Methods: (E-2-Benzoyl-3-(substituted phenylacrylonitriles (BPA analogs with a linear β-phenyl-α,β-unsaturated carbonyl scaffold were designed and synthesized as potential tyrosinase inhibitors. We evaluated their effects on cellular tyrosinase activity and melanin biosynthesis in murine B16F10 melanoma cells and their ability to inhibit mushroom tyrosinase activity. Results: BPA analogs exhibited inhibitory activity against mushroom tyrosinase. In particular, BPA13 significantly suppressed melanin biosynthesis and inhibited cellular tyrosinase activity in B16F10 cells in a dose-dependent manner. A docking study revealed that BPA13 had higher binding affinity for tyrosinase than kojic acid. Conclusion: BPA13, which possesses a linear β-phenyl-α,β-unsaturated carbonyl scaffold, is a potential candidate skin-whitening agent and treatment for diseases associated with hyperpigmentation. Keywords: (E-2-benzoyl-3-(substituted phenylacrylonitriles, melanogenesis, tyrosinase inhibitor

  15. Nickel(II Complexes of Hydrazone of Isoniazid and Their Magneto-Spectral, Electrochemical, Thermal and Antimicrobial Investigations

    Directory of Open Access Journals (Sweden)

    Surendra Prasad

    2008-01-01

    Full Text Available The synthesis of novel nickel(II complexes with new ligand derived from hydrazone of isoniazid has been reported. The complexes have general compositions [Ni(L2X2] or [Ni(L3](ClO42, where L = N-isonicotinamido-furfuraldimine (INH-FFL and X=Cl− or NCS−. The ligand hydrazone behaves as neutral bidentate (N and O donor through the carbonyl oxygen and azomethine nitrogen. On the basis of elemental analysis, molecular weight determinations, magnetic susceptibility/moment, thermogravimetric, electrochemical, and spectroscopic studies, the new complexes have been characterized with octahedral geometry. The antibacterial and antifungal studies of the present complexes show that they are moderate antibacterial and antifungal agents.

  16. Sensitive fluorescence probes for dihydrogen phosphonate anion based on calix[4]arene bearing naphthol-hydrazone groups

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    t-Butyl and t-pentylcalix[4]arenes bearing two 2-naphthol-1-hydrazone groups at the lower rim were synthesized,and showed excited-state intermolecular proton transfer fluorescent signal with basic anion.They are more sensitive to dihydrogen phosphate anion than to fluoride anion,although the latter has stronger basicity.Compared with t-butylcalix[4]arene bearing two 2-naphthol-1-hydrazone groups,t-pentylcalix[4]arenes derivative has a larger fluorescent difference between dihydrogen phosphate and fluoride anion.This finding may be used to analyze dihydrogen phosphate anion in the presence of fluoride anion and provide a new approach for designing fluorescence probes that are highly selective for H2PO4-.

  17. Synthesis, characterization and anticancer evaluation of novel tri-arm star shaped 1,3,5-triazine hydrazones

    Science.gov (United States)

    Machakanur, Shrinath S.; Patil, Basavaraj R.; Badiger, Dayananda S.; Bakale, Raghavendra P.; Gudasi, Kalagouda B.; Annie Bligh, S. W.

    2012-03-01

    A series of novel trisubstituted triazine hydrazones [N3C3(sbnd OC6H4-p-CHdbnd Nsbnd NHsbnd C(O)sbnd C6H4-p-X)3] (X = H, Br, Cl, F, OH, OCH3, CH3, NO2, NH2) were prepared by a three-fold condensation reaction of 2,4,6-tris(4-formylphenoxy)-1,3,5-triazine with p-substituted benzoic acid hydrazides [NH2sbnd NHsbnd C(O)sbnd C6H4-p-X] with excellent yields. The structures were confirmed by elemental analysis, FT-IR, 1H, 13C, 2D-HSQC NMR and mass spectrometry (MALDI-TOF). These derivatives bearing hydrolysable hydrazone linkages were evaluated for their invitro antiproliferative activity against the human liver carcinoma cell line (HepG2) and human cervix carcinoma cell line (HeLa).

  18. Chemical Recycling of Expanded Polystyrene Waste: Synthesis of Novel Functional Polystyrene-Hydrazone Surface for Phenol Removal

    OpenAIRE

    Siyal, Ali N.; Memon, Saima Q; Sajida Parveen; Asma Soomro; Mazhar I. Khaskheli; Khuhawar, M. Y.

    2013-01-01

    Expanded polystyrene (EPS) waste was chemically recycled to a novel functional polystyrene-hydrazone (PSH) surface by acetylation of polystyrene (PS) and then condensation with phenyl hydrazine. The synthesized surface was characterized by the FT-IR and elemental analysis. Synthesized novel functional PSH surface was successfully applied for the treatment of phenol-contaminated industrial wastewater by solid-phase extraction. Multivariant sorption optimization was achieved by factorial design...

  19. Synthesis and biological activity evaluation of hydrazone derivatives based on a Tröger's base skeleton

    Czech Academy of Sciences Publication Activity Database

    Kaplánek, R.; Havlík, M.; Dolenský, B.; Rak, J.; Džubák, P.; Konečný, P.; Hajdúch, M.; Králová, Jarmila; Král, V.

    2015-01-01

    Roč. 23, č. 7 (2015), s. 1651-1659. ISSN 0968-0896 R&D Projects: GA ČR(CZ) GAP303/11/1291 Grant ostatní: GA MŠk(CZ) EE2.3.30.0060; GA MŠk(CZ) LO1304 Institutional support: RVO:68378050 Keywords : Anticancer agents * Cancer treatment * Complexation studies * Hydrazone * Troger's base Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.793, year: 2014

  20. Effect on serum sex hormone levels, immune index of benzoyl peroxide combining with Hirudoid on acne vulgaris

    Institute of Scientific and Technical Information of China (English)

    Lin Li; Jie Sun; The authorsi-heng Yu; Yun-hao Hu

    2015-01-01

    Objective:To observe the effect on serum sex hormone levels, immune index of benzoyl peroxide combining with Hirudoid on acne vulgaris.Methods: 185 patients with acne vulgaris included in the study the authorsre divided into the observation group (85 cases) and the control group (80 cases), the observation group was given the treatment of benzoyl peroxide combining with Hirudoid, and the control group was treated with benzoyl peroxide. To observe the change of hormones (T, FSH, LH, E2) and immune indexes (IgG, IgA, IgM, C3, C4, IL-2, sIL-2R) after 1 month of treatment.Results: After treatment, IgG, C3, C4, IL-2 of the observation group the authorsre significantly different than those before trteatment(P0.05); After treatment, IgG, C3, C4, IL-2 level of two groups the authorsre statistically significant (P<0.05).Where the authorsre no significant difference on sex hormones betthe authorsen the two groups before and after treatment.Conclusion:Benzoyl peroxide combining with Hirudoid has certain effects on immune function for the patients with acne vulgaris, and may be related to therapeutic effect, but no obvious effect on sex hormone.

  1. Synthesis, Crystal Structures and Spectroscopic Properties of Triazine-Based Hydrazone Derivatives; A Comparative Experimental-Theoretical Study

    Directory of Open Access Journals (Sweden)

    Muhammad Nadeem Arshad

    2015-04-01

    Full Text Available We report here a comparative theoretical and experimental study of four triazine-based hydrazone derivatives. The hydrazones are synthesized by a three step process from commercially available benzil and thiosemicarbazide. The structures of all compounds were determined by using the UV-Vis., FT-IR, NMR (1H and 13C spectroscopic techniques and finally confirmed unequivocally by single crystal X-ray diffraction analysis. Experimental geometric parameters and spectroscopic properties of the triazine based hydrazones are compared with those obtained from density functional theory (DFT studies. The model developed here comprises of geometry optimization at B3LYP/6-31G (d, p level of DFT. Optimized geometric parameters of all four compounds showed excellent correlations with the results obtained from X-ray diffraction studies. The vibrational spectra show nice correlations with the experimental IR spectra. Moreover, the simulated absorption spectra also agree well with experimental results (within 10–20 nm. The molecular electrostatic potential (MEP mapped over the entire stabilized geometries of the compounds indicated their chemical reactivates. Furthermore, frontier molecular orbital (electronic properties and first hyperpolarizability (nonlinear optical response were also computed at the B3LYP/6-31G (d, p level of theory.

  2. Determination of organophosphorus pesticide residues in vegetables by an enzyme inhibition method using α-naphthyl acetate esterase extracted from wheat flour*

    OpenAIRE

    WANG, JUN-LIANG; Xia, Qing; Zhang, An-Ping; Hu, Xiao-Yan; Lin, Chun-mian

    2012-01-01

    The widespread use of organophosphorus pesticides (OPs) poses a great threat to human health and has made the detection of OP residues in food an important task, especially in view of the fact that easy and rapid detection methods are needed. Because OPs have inhibitory effects on the activity of α-naphthyl acetate esterase (ANAE) in plants, in this work we evaluated the possibility of detecting OPs in vegetables with ANAE extracted from commercial flour. The limits of detection (LODs) obtain...

  3. PPA-SiO2 Catalyzed Multi-component Synthesis of N-[α-(β-Hydroxy-α-naphthyl)(benzyl)]O-Alkyl Carbamate Derivatives

    Institute of Scientific and Technical Information of China (English)

    SHATERIAN,Hamid Reza; HOSSEINIAN,Asghar; GHASHANG,Majid

    2009-01-01

    Silica-supported polyphosphoric acid (PPA-SiO2) was found to be an efficient catalyst for the multi-component condensation reaction of benzaldehydes,2-naphthol,and methyl/benzyl carbamate to afford the corresponding N-[α-(β-hydroxy-α-naphthyl)(benzyl)]O-alkyl carbamate derivatives in good to excellent yields.This new approach consistently has the advantage of short reaction time,high conversions,clean reaction profiles,and simple experimental and work-up procedures.

  4. Synthesis and reactions of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one

    Directory of Open Access Journals (Sweden)

    NAGWA M.S. EL-DIN HARB

    1999-11-01

    Full Text Available The condensation of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one (3, prepared by the reaction of 6-[5,6,7,8-tetrahydro-2-naphthyl]-4,5-dihydropyridazin-3(2H-one (1 and anisaldehyde, with dimethyl sulphate, formaldehyde and acrylonitrile, and also the formation of the Mannich base, proceeded smoothly at the 2-position to give compounds 4,5,6,7, respectively. 4-p-Methoxybenzyl-3-chloro-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazine (9 was prepared in law yield by the action of phosphorus oxychloride on 3. The reaction of 9 with benzylamine, aniline and piperidine gave 10a,b,c, respectively. 4-p-Methoxybenzyl-6-[5,6,7,8-tetrahydro-2-napthyl]pyridazine-3(2H-thione (12 was prepared either by the action of thiourea on 9, or by the reaction of 3 with phosphorus pentasulphide. The reaction of these thiones with acrylonitrile, morpholine and piperidine to give 13 and 14 a,b, respectively, were also investigated.

  5. Liquid-liquid extraction of trivalent actinides and lanthanides with n-benzoyl-n-phenyl hydroxylamine

    International Nuclear Information System (INIS)

    Extraction of the trivalent actinides Am, Cm, Bk and Cf and the trivalent lanthanides Pm, Eu, Tb, Tm and Lu has been studied with N-benzoyl-N-phenyl hydroxylamine (HBPHA) in chloroform in the pH range 3.5-4.5. At pH 4.5 slopes of the log D vs. log [HBPHA] plots progressively decrease from 4 to 3 with increasing Z of the ions. Similar plots at pH 4.0 gave a uniform slope of 4 in all cases indicating the extraction of M (BPHA)3 HBPHA (M=An,Ln). In the pH ranges where this species is extracted log D vs. pH plots gave straight lines with slopes increasing from 2.0 to 2.7 with Z instead of the expected value of 3.0. Reasons for these abnormalities are discussed. (orig.)

  6. Comparative evaluation of retinoic acid, benzoyl peroxide and erythromycin lotion in acne vulgarils

    Directory of Open Access Journals (Sweden)

    Dogra A

    1993-01-01

    Full Text Available Ninety three patients suffering from acne vulgaris were treated with 0.05% retinoic acid (23 patients, 10% benzyoyl peroxide (24 patients, 2% erythromycin lotin (25 patients and 50% glycerine in methylated spirit (21 patients used as a control, for a period of 6 weeks. The patients were evaluated at 2 weeks and 6 weeks by spot counting of the lesions and diagrammatic representations. Good to excellent results were obtained in 69.6% of patients of erythromycin lotion. Retinoic acid was more effective in reducing noninflammatory lesions (75.2% whereas inflammatory lesions showed better response (73.6% with erythromycin lotion and benzoyl peroxide was almost equally effective in both types of lesions.

  7. Identification of Minor Benzoylated 4-Phenylcoumarins from a Mammea neurophylla Bark Extract

    Directory of Open Access Journals (Sweden)

    Bach Tai Dang

    2015-09-01

    Full Text Available Through dereplication analysis, seven known Mammea coumarins were identified in a fraction obtained from Mammea neurophylla dichloromethane bark extract selected for its ability to prevent advanced glycation end-product (AGE formation. Among them, a careful examination of the NMR dataset of pedilanthocoumarin B led to a structural revision. Inspection of LC-DAD-MSn chromatograms allowed us to predict the presence of four new compounds, which were further isolated. Using spectroscopic methods (1H-, 13C- and 2D-NMR, HRMS, UV, these compounds were identified as new benzoyl substituted 4-phenylcoumarins (iso-pedilanthocoumarin B and neurophyllol C and 4-(1-acetoxypropylcoumarins cyclo F (ochrocarpins H and I.

  8. Synthesis, structure and photophysical properties of a binuclear Zn(II) complex based on 8-hydroxyquinoline ligand with naphthyl unit

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Guozan, E-mail: yuanguozan@163.com [School of Chemistry and Chemical Engineering, Anhui University of Technology, Maanshan 243002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, Fujian (China); Shan, Weilong; Chen, Jiangbo; Tian, Yulan; Wang, Haitao [School of Chemistry and Chemical Engineering, Anhui University of Technology, Maanshan 243002 (China)

    2015-04-15

    A 2-substituted-8-hydroxyquinoline ligand (E)-2-[2-naphthyl-ethenyl]-8-hydroxyquinoline (HL) was synthesized and characterized by LC–MS, NMR spectroscopy, elemental analysis and single-crystal X-ray diffraction. Using a solvothermal method, a binuclear complex [Zn{sub 2}L{sub 4}] (1) was fabricated by self-assembly of Zn(II) ion with ligand HL. X-ray structural analysis shows that the binuclear Zn(II) units are linked into 1D chain along the b axis via aromatic stacking. The coordination assembly of zinc salt and HL in solutions was investigated by UV–vis and photoluminescence (PL). Additionally, we also studied the thermal stability and photophysical properties of (fluorescent emission and lifetime) complex 1. The experimental results show that the complex 1 emits yellow luminescence in the solid state. - Highlights: • Ligand HL and binuclear complex 1 were synthesized and characterized. • Complex 1 features a 2D network constructed by non-covalent interactions. • Complex 1 emits yellow luminescence in the solid state.

  9. Histological changes and impairment of liver mitochondrial bioenergetics after long-term treatment with α-naphthyl-isothiocyanate (ANIT)

    International Nuclear Information System (INIS)

    This study was designed to evaluate the effects of long-term treatment with α-naphthyl-isothiocyanate (ANIT) on liver histology and at the mitochondrial bioenergetic level. Since, ANIT has been used as a cholestatic agent and it has been pointed out that an impairment of mitochondrial function is a cause of hepatocyte dysfunction leading to cholestatic liver injury, serum markers of liver injury were measured and liver sections were analyzed in ANIT-treated rats (i.p. 80 mg/kg/weekx16 weeks). Mitochondrial parameters such as transmembrane potential, respiration, calcium capacity, alterations in permeability transition susceptibility and ATPase activity were monitored. Histologically, the most important features were the marked ductular proliferation, proliferation of mast cells and the presence of iron deposits in ANIT-treated liver. Mitochondria isolated from ANIT-treated rats showed no alterations in state 4 respiration, respiratory control ratio and ADP/O ratio, while state 3 respiration was significantly decreased. No changes were observed on transmembrane potential, but the repolarization rate was decreased in treated rats. Consistently with these data, there was a significant decrease in the ATPase activity of treated mitochondria. Associated with these parameters, mitochondria from treated animals exhibited increased susceptibility to mitochondrial permeability transition pore opening (lower calcium capacity). Since, human cholestatic liver disease progress slowly overtime, these data provide further insight into the role of mitochondrial dysfunction in the process

  10. Synthesis, structure and photophysical properties of a binuclear Zn(II) complex based on 8-hydroxyquinoline ligand with naphthyl unit

    International Nuclear Information System (INIS)

    A 2-substituted-8-hydroxyquinoline ligand (E)-2-[2-naphthyl-ethenyl]-8-hydroxyquinoline (HL) was synthesized and characterized by LC–MS, NMR spectroscopy, elemental analysis and single-crystal X-ray diffraction. Using a solvothermal method, a binuclear complex [Zn2L4] (1) was fabricated by self-assembly of Zn(II) ion with ligand HL. X-ray structural analysis shows that the binuclear Zn(II) units are linked into 1D chain along the b axis via aromatic stacking. The coordination assembly of zinc salt and HL in solutions was investigated by UV–vis and photoluminescence (PL). Additionally, we also studied the thermal stability and photophysical properties of (fluorescent emission and lifetime) complex 1. The experimental results show that the complex 1 emits yellow luminescence in the solid state. - Highlights: • Ligand HL and binuclear complex 1 were synthesized and characterized. • Complex 1 features a 2D network constructed by non-covalent interactions. • Complex 1 emits yellow luminescence in the solid state

  11. Thermoanalytical study of N{sub {alpha}}-benzoyl-L-argininate ethyl ester chloride

    Energy Technology Data Exchange (ETDEWEB)

    Fonseca, A.C. [Department of Chemical Engineering, University of Coimbra, Polo II, Pinhal de Marrocos, Coimbra 3030-790 (Portugal); Jarmelo, S. [Department of Chemical Engineering, University of Coimbra, Polo II, Pinhal de Marrocos, Coimbra 3030-790 (Portugal); Department of Chemistry, University of Coimbra, Coimbra 3004-535 (Portugal); Canotilho, J. [Faculty of Pharmacy, University of Coimbra, Polo das Ciencias da Saude, Azinhaga de Santa Comba, Coimbra 3000-548 (Portugal); Eusebio, M.E.S.; Fausto, R. [Department of Chemistry, University of Coimbra, Coimbra 3004-535 (Portugal); Gil, M.H.; Simoes, P.N. [Department of Chemical Engineering, University of Coimbra, Polo II, Pinhal de Marrocos, Coimbra 3030-790 (Portugal)

    2012-01-10

    Highlights: Black-Right-Pointing-Pointer Thermal analysis of crystalline N{sub {alpha}}-benzoyl-L-argininate ethyl ester chloride. Black-Right-Pointing-Pointer Characterization by STA, MDSC, PLTM, and HiRes-MTGA. Black-Right-Pointing-Pointer Non-isothermal kinetic analysis of the thermal decomposition. - Abstract: N{sub {alpha}}-benzoyl-L-argininate ethyl ester chloride (BAEEH{sup +}{center_dot}Cl{sup -}) has been used as a model drug in the development of polymeric delivery systems for peptides and proteins. In this study, crystalline BAEEH{sup +}{center_dot}Cl{sup -} was characterized by different thermoanalytical techniques. The main thermal events were identified by modulated differential scanning calorimetry (MDSC). Polarized light thermomicroscopy (PLTM) showed that no phase transitions but fusion occur before thermal decomposition. A crystalline phase could not be obtained from the melt in cooling/heating cycles between 150 Degree-Sign C and -150 Degree-Sign C, at 10 Degree-Sign C min{sup -1} scanning rate. The thermal stability and the non-isothermal kinetic analysis of the thermal decomposition were studied by conventional and high resolution modulated thermogravimetric analysis (HiRes-MTGA). Depending on the conditions of the study, the decomposition starts in the range from 197 Degree-Sign C (HiRes-MTGA at {phi} = 2 Degree-Sign C min{sup -1}) to 261 Degree-Sign C (TGA at 20 Degree-Sign C min{sup -1}). It was found that the first stage of the decomposition process can be described by the kinetic triplet E{sub a} = 142 kJ mol{sup -1}, A = 1.86 Multiplication-Sign 10{sup 11} s{sup -1}, and f({alpha}) = (1 - {alpha}){sup 2.78}.

  12. Thermoanalytical study of Nα-benzoyl-L-argininate ethyl ester chloride

    International Nuclear Information System (INIS)

    Highlights: ► Thermal analysis of crystalline Nα-benzoyl-L-argininate ethyl ester chloride. ► Characterization by STA, MDSC, PLTM, and HiRes-MTGA. ► Non-isothermal kinetic analysis of the thermal decomposition. - Abstract: Nα-benzoyl-L-argininate ethyl ester chloride (BAEEH+·Cl−) has been used as a model drug in the development of polymeric delivery systems for peptides and proteins. In this study, crystalline BAEEH+·Cl− was characterized by different thermoanalytical techniques. The main thermal events were identified by modulated differential scanning calorimetry (MDSC). Polarized light thermomicroscopy (PLTM) showed that no phase transitions but fusion occur before thermal decomposition. A crystalline phase could not be obtained from the melt in cooling/heating cycles between 150 °C and −150 °C, at 10 °C min−1 scanning rate. The thermal stability and the non-isothermal kinetic analysis of the thermal decomposition were studied by conventional and high resolution modulated thermogravimetric analysis (HiRes-MTGA). Depending on the conditions of the study, the decomposition starts in the range from 197 °C (HiRes-MTGA at φ = 2 °C min−1) to 261 °C (TGA at 20 °C min−1). It was found that the first stage of the decomposition process can be described by the kinetic triplet Ea = 142 kJ mol−1, A = 1.86 × 1011 s−1, and f(α) = (1 − α)2.78.

  13. Potentiometric and spectrophotometric studies of the complexation of Schiff-base hydrazones containing the pyrimidine moiety

    Directory of Open Access Journals (Sweden)

    M. SHEBL

    2003-10-01

    Full Text Available Three Schiff-base hydrazones (ONN – donors were prepared by condensation of 2-amino-4-hydrazino-6-methylpyrimidine with 2-hydroxyacetophenone, 2-methoxybenzaldehyde and diacetyl to yield 2-OHAHP, 2-OMeBHP and DHP, respectively. The structures of these ligands were elucidated by elemental analysis, UV, IR, 1H-NMR and mass spectra. The metal–ligand stability constants of Mn2+, Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, UO22+ and Th4+ chelates were determined potentiometrically in two different media (75 % (v/v dioxane–water and ethanol–water at 283, 293, 303 and 313 K at an ionic strength of 0.05 M (KNO3. The thermodynamic parameters of the 1:1 and 1:2 complexes were evaluated and are discussed. The dissociation constants of 2-OHAHP, 2-OMeBHP and DHP ligands and the stability constants of Co2+, Ni2+ and Cu2+ with 2-OHAHP were determined spectrophotometrically in 75 % (v/v dioxane–water.

  14. Radiation induced conductivity of polycarbonate doped with different concentrations of aromatic hydrazone DEH

    Science.gov (United States)

    Vladimir, Saenko; Novikov, Lev; Tyutnev, Andrey

    Radiation induced conductivity (RIC) of polymers widely used on present-day spacecraft plays is an important factor affecting their charging by the hot plasma of the Earth’s magnetosphere. As a result, researchers pay special attention to laboratory investigations of RIC in polymers excited by 10 -100 keV electrons prevailing in the hot magnetospheric plasma, including auroral radiation. Due to fluctuating fluxes of plasma electrons and especially of auroral electrons, it is very important to know how RIC depends on time. In our report we present RIC results observed in polycarbonate (PC) molecularly doped with aromatic hydrazone DEH (10 to 30 mas. percent) under continuous irradiation with 50 keV electrons. It has been found that RIC behavior in this material differs markedly from what we observed earlier in most of the polymers. After beginning of the stepwise irradiation, the RIC of PC+DEH rises fast to the quasistationary level but unlike common polymers, does not fall by an order of magnitude, instead it starts to increase further thus causing the accumulating space charge to decrease. This fact combined with the confirmed high radiation and temperature tolerance allows us to recommend this material for application on the spacecraft outer surface and specifically, as a thermal blanket.

  15. Coordination diversity of new mononucleating hydrazone in 3d metal complexes: Synthesis, characterization and structural studies

    Directory of Open Access Journals (Sweden)

    RAJESH S. BALIGAR

    2006-12-01

    Full Text Available The mononucleating hydrazone ligand LH3, a condensation product of salicyloylhydrazine and (2-formylphenoxyacetic acid, was synthesized and its coordination behavior with first row transition metal(II ions was investigated by isolating and elucidating the structure of the complexes using elemental analysis, conductivity and magnetic susceptibility measurements, as well as IR, 1H-NMR, electronic and EPR spectral techniques. The ligand forms mononuclear metal(II complexes of the type [CoLH(H2O2], [NiLH(H2O2, [CuLH] and [ZnLH]. The ligand field parameters, Dq, B and b values, in the case of the cobalt and nickel complexes support not only the octahedral geometry around the metal ion, but also imply the covalent nature of the bonding in the complexes. The EPR study revealed the presence of a spin exchange interaction in the solid copper complex and the covalent nature of the bonding. The 1H-NMR study of the zinc(II complex indicated the non-involvement of the COOH group in the coordination. The physico-chemical study supports for the presence of octahedral geometry around cobalt(II, nickel(II and tetrahedral geometry around copper(II and zinc(II ions.

  16. Determination of the dissociation constants of some p-substituted aromatic hydrazones

    International Nuclear Information System (INIS)

    The acid-base behavior of five p-substituted aromatic hydrazones has been studied, using UV spectrophotometric method. The influence of the acidity of the medium on the absorption spectra is followed in aqueous sodium hydroxide solutions in ph region from 7 to 14. The measurements are performed at room temperature, and at ionic strength of 0.1, 0.25 and 0.5 mol dm-3. A batochromic shift of the absorption band that appears in neutral media is observed, when ph is up to 7. It suggests that the dissociation process of the amide and hydroxyl group takes place. Deprotonation enthalpies and total energy values are calculated by using the semiempirical methods A M1 and P M3. Using the changes in the UV spectra with ph of the solution, the determination of dissociation constants, pKBH, at three different ionic strengths, as well as, the thermodynamic dissociation constants at zero ionic strength, is performed. In order to obtain more precise results, the calculations are made from the absorbance values at four selected wavelengths. Furthermore, the pKBH values were determined graphically from the intercept of the dependence of log I on ph. The results showed that the numerically calculated pKBH values are identical to those graphically obtained. (Author)

  17. Synthesis, characterization and studies on the nonlinear optical parameters of hydrazones

    Science.gov (United States)

    Naseema, K.; Sujith, K. V.; Manjunatha, K. B.; Kalluraya, Balakrishna; Umesh, G.; Rao, Vijayalakshmi

    2010-07-01

    Three hydrazones, 2-(4-methylphenoxy)- N'-[(1E)-(4-nitrophenyl)methylene]acetohydrazide (compound-1), 2-(4-methylphenoxy)- N'-[(1E)-(4-methylphenyl)methylene]acetohydrazide ((compound-2) and N'-{(1E)-[4-(dimethylamino)phenyl]methylene}-2-(4-ethylphenoxy) acetohydrazide(compound-3) were synthesized and their third order nonlinear optical properties were investigated using a single beam z-scan technique with nanosecond laser pulses at 532 nm. Open aperture data obtained from the three compounds indicates two photon absorption at this wavelength. The nonlinear refractive index n2, the nonlinear absorption coefficient β, the magnitude of the effective third order susceptibility χ(3), the second order hyperpolarizability γh and the coupling factor ρ have been estimated. The values obtained are comparable with the values obtained for 4-methoxy chalcone derivatives and dibenzylidene acetone derivatives. Among the compounds studied, compounds-1 and 3 exhibited the better optical power limiting behaviour at 532 nm. Our studies suggest that compounds-1, 2 and 3 are potential candidates for optical device applications such as optical limiters and optical switches.

  18. Synthesis, characterization and density functional theory study of low cost hydrazone sensitizers

    KAUST Repository

    G. Al-Sehemi, A.

    2015-01-18

    © 2015 Chemical Society of Ethiopia The 2-{4-[2-benzylidenehydrazino]phenyl}ethylene-1,1,2-tricarbonitrile (System 1), 2-{4-[2-(1- naphthylmethylene)hydrazino]phenyl}ethylene-1,1,2-tricarbonitrile (System 2) and 2-{4-[2-(9-anthrylmethylene)- hydrazino]phenyl}ethylene-1,1,2-tricarbonitrile (System 3) were synthesized by direct tricyanovinylation of hydrazones. The bathochromic shift in absorption spectra has been observed by increasing the solvent polarity. The FTIR spectra of these new dyes exhibited three important absorption bands. The first band centered near 3260 cm-1 in System 1 while 3208 cm-1 and 3211 cm-1 in System 2 and System 3 for the vNH absorption, respectively. The second band is a sharp absorption band in the region of 2212-2209 cm-1, which was attributed to the cyano group absorption. The third is an absorption band in the region of 1611-1603 cm-1 ascribed for the C=N. Density functional theory (DFT) calculation of relative energies, relative enthalpies and free energies shows that E isomers are the most stable except System 3 in which the most stable is Z isomers. The conformational energy profile shows two maxima near (-90 and 90°) while three local minima observed at (-180, 0 and 180) for N1-N2-C1-C2 torsional angle. The highest occupied molecular orbitals (HOMOs) are localized on the whole molecules while lowest unoccupied molecular orbitals (LUMOs) are distributed on the tricarbonitrile.

  19. Investigation into the hypersensitive transitions of Ln(III)-(1-phenyl-3-methyl-4-benzoyl pyrazolone-5) anthranilic acid and (1-phenyl-3-methyl-4-benzoyl-pyrazolone-5) aminoantipyrine complexes-II

    International Nuclear Information System (INIS)

    (1-phenyl-3-methy1-4-benzoyl pyrazolone-5) anthranilic acid (PMBAA) and (1-phenyl-3-methyl-4-benzoyl-pyrazolone-5) amino-antipyrine (PMBAAP) form complexes with lanthanides of the type [Ln(PMBAA)2NO3] and (Ln(PMBAAP)3] where Ln = La, Pr, Nd, Sm, Eu, Gd, Tb, Dy and Y. These compounds have been characterized from physico-chemical studies. The electronic spectra of the Nd(III) complexes have been studied in detail to investigate the phenomenon of hypersensitivity with respect to the coordination environment and solvent medium. In these compounds solvents do play a significant role to cause variation in hypersensitivity. In general Nd(III) PMBAA complexes showed greater hypersensitivity than the Nd(III) PMBAAP complexes. IR and NMR have also been interpreted. (author). 13 refs., 4 tabs

  20. Antimicrobial and antioxidant screening of N¢-substituted sulphonyl and benzoyl derivatives of 4-Pyridine carboxylic acid hydrazide.

    Science.gov (United States)

    Naeem, Sabahat; Akhtar, Shamim; Asghar, Nadia; Sherwani, Sikander Khan; Mushtaq, Nousheen; Kamil, Arfa; Zafar, Shaista; Arif, Mohammad; Saify, Zafar Saeed

    2015-11-01

    In this research program, the antibacterial, antifungal and antioxidant activities of six N'-substituted sulfonyl and benzoyl derivatives of lead molecule PCH were reported. Out of these compounds, sulphonyl derivatives 2,3 and benzoyl derivative 5 showed moderate to good activity against different strains of gram-positive and gram-negative bacteria including B. cereus, B. subtilis, B. thruingiensis and S. pyogenes, S. fecalis and E. coli ATCC 8739. Moreover, upon antifungal screening, the compound, N¢-[(2,4,6-trimethylbenzene) sulfonyl]pyridine-4-carbohydrazide possessed good antifungal activity against Candida species, a causative agent of systemic fungal infections. Antioxidant study demonstrated more than 50% inhibition in DPPH assay for sulphonyl derivative 2 indicating its potential as antioxidant while the other derivatives expressed low level of radical scavenging property. PMID:26639506

  1. Computational and spectroscopic studies of the imidazole-fused phenanthroline derivatives containing phenyl, naphthyl, and anthryl groups

    Science.gov (United States)

    Wang, Jinglan; Xu, Shengxian; Zhao, Feng; Xia, Hongying; Wang, Yibo

    2016-03-01

    Three N,N-bidentate ligands, 2-phenyl-1H-imidazo[4,5-f][1,10]phenanthroline (1), 2-(2-naphyl)-1H-imidazo[4,5-f]phenanthroline (2), and 2-(2-anthryl)-1H-imidazo[4,5-f]phenanthroline (3) have been synthesized and characterized. Effects of aryl subsistiuents (phenyl, naphthyl, and anthryl) on the photophysical properties of these ligands in solution have been studied. Ligand 1 exhibit the main absorption band at 283 nm with the shoulder bands at 300-350 nm and these bands are assigned as the typical π→π*(imPhen) state (imPhen = 1H-imidazo[4,5-f][1,10]phenanthroline). A similar absorption spectrum was also observed in the case of 2, in which the charge transfer (CT) state should be considered. 3 shows the slightly different absorption properties compared to that of 1 and 2. The highest-lying absorption band at 257 nm is assigned as a mixed π→π*(imPhen)/π→π*(Anth) (Anth = anthracene) state. Additionally, the characteristic absorption band of anthryl group with three vibronic bands at 352, 367, and 386 nm also observed in the visible region range from 340 to 400 nm. 1 shows the typical ligand-centered 1π→π* emission, while 2 and 3 emit from the mixed 1π→π*/CT states. Density functional theory (DFT) and time-dependent density functional theory (TDDFT) were employed to rationalize the photophysical properties of these ligands studied. The theoretical data confirm the assignment of the experimental absorption spectra and the nature of the emitting states.

  2. EFIKASI LARVASIDA BERBAHAN AKTIF BENZOYL PHENIL UREA SEBAGAI INSECT GROWTH REGULATOR TERHADAP LARVA Culex quinquefasciatus DI LABORATORIUM

    Directory of Open Access Journals (Sweden)

    Siti Alfiah

    2014-06-01

    Full Text Available This study was conducted to determine the efficacy of an insect growth regulator (IGRbenzoyl phenil urea against Culex quinquefasciatus larvae, laboratory scale trial. The researchused seven concentrations of IGR, were evaluated 0,5 ; 1 ; 2 ; 2,5 ; 3 and 5 ppm and untreatedcontrol, using 4 replications (20 larvae each. The result showed that 0,5 ppm of the benzoylphenil urea could kill more 90% of Cx. quinquefasciatus larvae in 5 days, while concentrations 1; 2 ; 2,5 and 3 ppm in 4 days, and concentration 5 ppm in 3 days. The result was also revealedthat LC50 and LC90 0,57 and 23,2 ppm. Mosquito larvae mortalities were showed statisticallydifferent among concentrations (p < 0,05.Key words : Efficacy, benzoyl phenil urea, Culex quinquefasciatus Penelitian untuk mengetahui efikasi insect growth regulator (IGR benzoyl phenil ureaterhadap larva Culex quinquefasciatus telah dilakukan. Penelitian menggunakan 7 konsentrasipengujian yaitu 0,5 ppm, 1 ppm, 2 ppm, 2,5 ppm, 3 ppm, 5 ppm dan kontrol. Setiap konsentrasimenggunakan 4 kali pengulangan. Hasil menunjukkan bahwa larvasida benzoyl phenil ureamembunuh lebih dari 90% larva Cx. quinquefasciatus dengan konsentrasi 0,5 ppm dalam 5 hari,konsentrasi 1 ; 2 ; 2,5 dan 3 ppm dalam waktu 4 hari dan konsentrasi 5 ppm dalam waktu 3 hari.Konsentrasi yang diperlukan untuk membunuh 50% (LC50 dan 90% (LC90 larva uji adalah 0,57ppm dan 23,2 ppm. Uji analisis varian memberikan hasil bahwa ada perbedaan bermaknakematian larva antar konsentrasi pada taraf nyata 5%.Kata kunci : Efikasi, benzoyl phenil urea, Culex quinquefasciatus

  3. Multicenter study to evaluate efficacy and irritation potential of benzoyl peroxide 4% cream in hydrophase base (Brevoxyl in acne vulgaris

    Directory of Open Access Journals (Sweden)

    Sawleshwarkar S

    2003-01-01

    Full Text Available In this multicenter, open, non-comparative study, the efficacy and irritation potential of 4% benzoyl peroxide cream in hydrophase base (Brevoxyl was evaluated for the treatment of acne vulgaris. All evaluable patients (n=567 received treatment with 4% benzoyl peroxide cream in hydrophase base for six weeks. The investigators evaluated the patients at baseline and at 1,2,4 & 6 weeks. Patients also rated their improvement and adverse effects. Doctor′s assessment showed that at the end of 6′h week 85.6% had good to very good effect of the treatment. The profile of side effects observed by doctors revealed that 53.8% of total patients did not have any irritation whereas only 11.6% had moderate to severe irritation. 53.8% of patients did not report any irritation: 41.4% had some irritation whereas only 4.8% patients reported troublesome irritation. A satisfactory response was reported as ear;y as two weeks and most of the patients had a very satisfactory response after six weeks and were willing to continue the treatment. This supports the theory that the hydrophase formulation in ′Brevoxyl helped to enhance efficacy and decrease the irritation associated with use of benzoyl peroxide.

  4. Synthesis characterization and toxicity of lanthanide complexes with schiff bases derived from S-benzoyl dithiocarbazate and aldehydes

    International Nuclear Information System (INIS)

    New O:N:S and N:S donor ligands namely, S-benzoyl-N-(o-hydroxybenzaldehyde) dithiocarbazate, S-benzoyl-N-(N,N-dimethylaminobenzaldehyde ) dithiocarbazate, S-benzoyl-N(N-thiophene-2-aldehyde) dithiocarbazate and their complexes with La(III), Ce(III), Pr(III), Nd(III), Sm(III), Gd(III), Tb(III), Dy(III), Ho(III), Er(III), Yb(III), and Lu(III) have been synthesized and characterized on the basis of elemental analysis, IR, NMR and electronic spectroscopy. The nephelauxetic effect(1-βoverlined), bonding parameter, βoverlined, bsup(1/2) and Sinha covalency parameter δ, have been calculated. Their positive values indicate covalent nature of metal-ligand bond which is also supported by their molar conductances measured in nitrobenzene. Magnetic moment values exhibit paramagnetic nature of the complexes. Log K,ΔG, ΔH and ΔS values have also been ca lculated. Toxicity of the compounds has been evaluated against cockroaches and fungi(Aspergillus flavus and A. niger). The LD50 and % inhibition values demonstrate greater efficacy of the complexes than that of the free bases. (author). 4 tabs., 12 refs

  5. Coordination polymers of La(III) acetate with terephthalaldehyde bis isonicotinic acid hydrazone (Paper No. AL-12)

    International Nuclear Information System (INIS)

    Polymerization reactions involving the formation of schiff base metal complexes by condensation have been described. Metal complexes of schiff bases of hyrazides with aldehydes and ketones have been of special interest in recent years, particularly in the context of therapeutic value of hydrazide and hydrazone. The coordination occurs both in keto as well as in enolic form of ligands with metal ions. Coordination polymers of 3-d series have been extensively studied but less attention has been paid on rare earths polymeric complexes. The synthesis and characterization of lanthanide (La, Pr, Nd, Sr and Gd) acetate complexes with a schiff base derived from terephthalaldehyde and isonicotinic acidhydrazide are reported. (author)

  6. Synthesis, Spectral and Thermal Investigations of Some Oxovanadium(IV) Complexes of Hydrazones of Isonicotinic Acid Hydrazide

    OpenAIRE

    Agarwal, Ram K.; Singh, Lakshman

    2005-01-01

    A new series of 12 complexes of oxovanadium(IV) with hydrazones of isonicotinic acid hydrazide, namely N-isonicotinamido-3',4',5'-trimethoxybenzalaldimine (INH-TMB) and N-isonicotinamido-2'-furanaldimine (INH-FUR) with the general formula VOX2.nL (X = Cl, Br, I, NCS, NO3, n = 1; X = ClO4, n = 2; L = INH-TMB or INH-FUR) were synthesized and characterized on the basis of analytical, conductance, molecular weight, magnetic moment, infrared and electronic spectral data....

  7. Synthesis, Characterization of α-Oxopentanedioic Acid-Isonicotinoyl Hydrazone Rare Earth-Complexes and Relaxivity of Gd-complex

    Institute of Scientific and Technical Information of China (English)

    杨正银; 杨汝栋

    2004-01-01

    α-Oxopentanedioic acid isonicotinoyl hydrazone (H2L) and its five rare earth complexes were synthesized with a view to further investigating MRI activities of the polycarboxylic Schiff base complexes. The complexes were characterized on the basis of elemental analyses, IR, UV, 1H NMR spectra and thermal analyses. The general formula of the complexes is [Ln(HL)(H2O)2]Cl2·H2O (where Ln(Ⅲ)=La, Pr, Nd, Eu and Gd). In addition, the relaxivity (R1) of the Gd-complex was determined by INVREC Au program.

  8. Enantioselective Rhodium(I) Donor Carbenoid-Mediated Cascade Triggered by a Base-Free Decomposition of Arylsulfonyl Hydrazones.

    Science.gov (United States)

    Torres, Òscar; Parella, Teodor; Solà, Miquel; Roglans, Anna; Pla-Quintana, Anna

    2015-11-01

    The reaction of diyne arylsulfonyl hydrazone substrates under rhodium(I)/BINAP catalysis gives access to sulfonated azacyclic frameworks in a highly enantioselective manner. This new cascade process considerably increases the molecular complexity by generating two C-C bonds, one C-S bond, and one C-H bond. Theoretical calculations, competitive experiments, and deuterium labeling have jointly been used to propose a mechanism that accounts for the reaction. The mechanism involves the formation of vinyl rhodium carbenoids, hydride migratory insertion, and intermolecular stereoselective nucleophilic attack. The last two steps are the key to the stereoselectivity of the process. PMID:26397988

  9. Polymer complexes. XLXI. Supramolecular spectral studies on metal-ligand bonding of novel rhodanine sulphadrugs hydrazone

    International Nuclear Information System (INIS)

    Graphical abstract: The ESR spectra of copper complexes in powder form show a broad signal with values in order g|| > g( > ge (2.0023). The value of covalency factor β and orbital reduction factor K accounts for the covalent nature of the complexes. -- Abstract: Novel polymeric complexes with 5-sulphadiazineazo-3-phenyl-2-thioxo-4-thiazolidine (HL1), 5-sulphamethazineazo-3-phenyl-2-thioxo-4-thiazolidine (HL2) and 5-sulphamethoxazoleazo-3-phenyl-2-thioxo-4-thiazolidine (HL3) and various anions were prepared. Structural and spectroscopic properties have been studied on the basis of elemental analyses, infrared spectra, 1HNMR spectra, electronic spectra, magnetic measurements and ESR. IR and 1H NMR studies reveal that the ligands (HLn) exists in the tautomeric enol/hydrazo form in both states with intramolecular hydrogen bonding. The analytical data and the molar conductance measurements of the polymeric complexes reveal that three molecules of the ligand and four/two(Cl/SO4) of the anions are coordinated to the two metal atoms in all complexes. The infrared spectra of the ligands and their polymeric complexes, confirmed that the ligands coordinate to Cu(II) as a neutral and tetradentate via NH(hydrazone), oxygen of the carbonyl group (CO), nitrogen of the NH(3-phenylamine) and thion sulphur (CS) group. All the polymer complexes were found to have magnetic moments corresponding to one unpaired electrons. The ESR (g|| and gperpendicular) and bonding α2 parameters of the copper ion were greatly affected by substituting several groups position of ring of sulphadrug. The ESR spectra of copper complexes in powder form show a broad signal with values in order g|| > gperpendicular > ge (2.0023). The value of covalency factor β and orbital reduction factor K accounts for the covalent nature of the complexes.

  10. Bivalent transition metal complexes of ONO donor hydrazone ligand: Synthesis, structural characterization and antimicrobial activity.

    Science.gov (United States)

    Bhaskar, Ravindra; Salunkhe, Nilesh; Yaul, Amit; Aswar, Anand

    2015-12-01

    Mononuclear transition metal complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with a new hydrazone ligand derived from pyrazine-2-carbohydrazide and 2-hydroxyacetophenone have been synthesized. The isolated complexes were characterized by elemental analysis, spectral and analytical methods including elemental analyses, IR, diffuse reflectance, (1)H-NMR, mass spectra, molar conductance, magnetic moment, ESR, XRD, TG and SEM analysis. From the elemental analyses data, the stoichiometry of the complexes was found to be 1:1 (metal:ligand) having the general formulae [M(HL)(Cl)(H2O)2], [M=Mn(II), Co(II), Ni(II) and Cu(II)] and [M(L)(H2O)], [M=Zn(II) and Cd(II)]. The molar conductance values indicate the nonelectrolytic nature of metal complexes. The IR spectral data suggest that the ligand behaves as tridentate moiety with ONO donor atoms sequence towards central metal ion. The Mn(II), Co(II), Ni(II) and Cu(II) complexes have been assigned a monomeric octahedral geometry whereas tetrahedral to Zn(II) and Cd(II) complexes. The antibacterial and antifungal activities of the ligand and its metal complexes were studied against bacterial species Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Bacillus subtilis, Enterococcus faecalis and Streptococcus pyogenes and fungi Candida albicans, Aspergillus niger and Aspergillus clavatus. The activity data show that the metal complexes have a promising biological activity comparable with the parent ligand against all bacterial and fungal species. PMID:26163785

  11. Purification of benzoyl-mercapto-acetyl-tri-glycine and ethyl cysteinate dimer complemented with biological evaluations

    International Nuclear Information System (INIS)

    Purification of benzoyl-mercaptoacetyl triglycine (MAG3) and ethyl cysteinate dimer (L,L-ECD) has been conducted through fractionated recrystallization of its impurities and isomers; biological behavior of the main isomers has been evaluated through biological distribution in mice. Chemical purity of synthesized MAG3 is 69,9%; after purification, 98, 12% is obtained from the compound with adequate biological distribution; fusion points range between 194 and 196oC before and after purification; recrystallization yields is 12%. Radiochemical purity of testing lot is 98%. In biological evaluations conducted in mice, injection dose percentages for the purest one, after 5 minutes, is 31,20% in kidneys and 1,14% in the liver. Chemical purity of synthesized ECD is 80,29%; after purification, 98,76% is obtained from the isomer with adequate biological activity; fusion points range between 195 and 197oC; yield percentage in recrystallization is 29%. radiochemical purity of testing lot is 97%; in biological evaluations conducted in mice, injection dose percentages for the purest one, after 5 minutes, is 1,37% in the brain, 25,70% in the liver and 13,40% in kidneys

  12. Polymeric micellar nanocarriers of benzoyl peroxide as potential follicular targeting approach for acne treatment.

    Science.gov (United States)

    Kahraman, Emine; Özhan, Gül; Özsoy, Yıldız; Güngör, Sevgi

    2016-10-01

    The aim of this work was to optimize polymeric nano-sized micellar carriers of the anti-acne compound benzoyl peroxide (BPO) and to examine the ability of these carriers to deposit into hair follicles with the objective of improving skin delivery of BPO. BPO loaded polymeric micelles composed of Pluronic(®) F127 were prepared by the thin film hydration method and characterized in terms of size, loading capacity, morphology and physical stability. The optimized micelle formulation was then selected for skin delivery studies. The penetration of BPO loaded micellar carriers into skin and skin appendages across full thickness porcine skin was examined in vitro. Confocal microscopy images confirmed the penetration of Nile Red into hair follicles, which was loaded into micellar carriers as a model fluorescent compound. The relative safety of the polymeric micelles was evaluated with the MTT viability test using mouse embryonic fibroblasts. The results indicated that nano-sized polymeric micelles of BPO composed of Pluronic(®) F127 offer a potential approach to enhance skin delivery of BPO and that targeting of micelles into hair follicles may be an effective and safe acne treatment. PMID:27434156

  13. Red-phosphorescent OLEDs employing iridium (III) complexes based on 5-benzoyl-2-phenylpyridine derivatives

    International Nuclear Information System (INIS)

    A series of red-phosphorescent iridium (III) complexes 1-4 based on 5-benzoyl-2-phenylpyridine derivatives was synthesized. Their photophysical and electrophosphorescent properties were investigated. Multilayered OLEDs were fabricated with a device structure ITO/4,4',4''-tris(N-(naphtalen-2-yl)-N-phenyl-amino)triphenylamine (60 nm)/4,4'-bis(N-naphtylphenylamino)biphenyl (20 nm)/Ir(III) complexes (8%) doped in 4,4'-N,N'-dicarbazolebiphenyl (30 nm)/2,9-Dimethyl-4,7-diphenyl-1,10-phenanthroline (10 nm)/tris(8-hydroxyquinolinyl)aluminum(III) (20 nm)/Liq (2 nm)/Al (100 nm). All devices exhibited efficient red emissions. Among those, in a device containing iridium complex 1 dopant, the maximum luminance was 14200 cd/m2 at 14.0 V. Also, its luminous, power, and quantum efficiency were 10.40 cd/A, 3.44 lm/W and 9.21% at 20 mA/cm2, respectively. The peak wavelength of the electroluminescence was 607 nm, with CIE coordinates of (0.615, 0.383) at 12.0 V, and the device also showed a stable color chromaticity with various voltages.

  14. Structural, spectroscopic and quantum chemical studies of acetyl hydrazone oxime and its palladium(II) and platinum(II) complexes

    Science.gov (United States)

    Kaya, Yunus; Icsel, Ceyda; Yilmaz, Veysel T.; Buyukgungor, Orhan

    2015-09-01

    Acetyl hydrazone oxime, [(1E,2E)-2-(hydroxyimino)-1-phenylethylidene]acetohydrazone (hipeahH2) and its palladium(II) and platinum(II) complexes, [M(hipeahH)2] (M = PdII and PtII), have been synthesized and characterized by elemental analysis, UV-vis IR, NMR and LC-MS techniques. X-ray diffraction analysis of [Pd(hipeahH)2] shows that the two hipeahH2 ligands are not equal; one of the ligands loses the hydrazone proton, while the other one loses the oxime proton, resulting in a different coordination behavior to form five- and six-membered chelate rings. The molecular geometries from X-ray experiments in the ground state were compared using the density functional theory (DFT) with the B3LYP method combined with the 6-311++G(d,p) basis set for the ligand and the LanL2DZ basis set for the complexes. Comprehensive theoretical and experimental structural studies on the molecule have been carried out by FT-IR, NMR and UV-vis spectrometry. In addition, the isomer studies of ligand and its complexes were made by DFT.

  15. Potential Amoebicidal Activity of Hydrazone Derivatives: Synthesis, Characterization, Electrochemical Behavior, Theoretical Study and Evaluation of the Biological Activity

    Directory of Open Access Journals (Sweden)

    Yanis Toledano-Magaña

    2015-05-01

    Full Text Available Four new hydrazones were synthesized by the condensation of the selected hydrazine and the appropriate nitrobenzaldehyde. A complete characterization was done employing 1H- and 13C-NMR, electrochemical techniques and theoretical studies. After the characterization and electrochemical analysis of each compound, amoebicidal activity was tested in vitro against the HM1:IMSS strain of Entamoeba histolytica. The results showed the influence of the nitrobenzene group and the hydrazone linkage on the amoebicidal activity. meta-Nitro substituted compound 2 presents a promising amoebicidal activity with an IC50 = 0.84 μM, which represents a 7-fold increase in cell growth inhibition potency with respect to metronidazole (IC50 = 6.3 μM. Compounds 1, 3, and 4 show decreased amoebicidal activity, with IC50 values of 7, 75 and 23 µM, respectively, as a function of the nitro group position on the aromatic ring. The observed differences in the biological activity could be explained not only by the redox potential of the molecules, but also by their capacity to participate in the formation of intra- and intermolecular hydrogen bonds. Redox potentials as well as the amoebicidal activity can be described with parameters obtained from the DFT analysis.

  16. Antimicrobial screening and one-pot synthesis of 4-(substituted-anilinomethyl-3-(2-naphthyl-1-phenyl-1H-pyrazole derivatives

    Directory of Open Access Journals (Sweden)

    Neelima Goel

    2014-01-01

    Full Text Available Aim: Synthesis of series of 4-(substituted-anilinomethyl-3-(2-naphthyl-1-phenyl-1H-pyrazole derivatives (4a-4k and their in vitro antifungal and antibacterial screening. Materials and Methods: A series of compounds (4a-4k was synthesized through direct reductive amination of 3-(naphthalen-2-yl-1-phenyl-1H-pyrazole-4-carbaldehyde with various substituted aromatic amines using NaBH 4 in the presence of I 2 as reducing agent. The reaction was carried out in anhydrous methanol under neutral conditions at room temperature. The structures of synthesized compounds (4a-4k were established on the basis of IR, 1 H and 13 C-NMR, and mass spectral data. Results: All 4-(substituted-anilinomethyl-3-(2-naphthyl-1-phenyl-1H-pyrazole derivatives (4a-4k were tested in vitro for antifungal and antibacterial activities against different fungal and bacterial strains. Most of the compounds exhibited considerable antifungal activity, but poor antibacterial activity against the test strains. Conclusion: In the series compound 4e, 4g, 4j, and 4k, showed excellent antifungal activity against the fungal strain Aspergillus niger (MTCC 281 and Aspergillus flavus MTCC 277 (% inhibition in the range of 47.7-58.9.

  17. Simple and fast fluorescence detection of benzoyl peroxide in wheat flour by N-methoxy rhodamine-6G spirolactam based on consecutive chemical reactions

    International Nuclear Information System (INIS)

    Graphical abstract: A simple and fast method for fluorescence detection of benzoyl peroxide in wheat flour by N-methoxy rhodamine-6G spirolactam (1) is proposed based on consecutive chemical reactions. Highlights: ► Benzoyl peroxide can oxidize Fe2+ into Fe3+. ► Fe3+ selectively induces the opening of rhodamine spirolactam ring. ► The two reactions led to the development of a new fluorescent method for benzoyl peroxide. ► The method is simple and fast, and is used to detect benzoyl peroxide in wheat flour. - Abstract: Benzoyl peroxide (BPO) as a brightener is often added to wheat flour, and excessive use of this food additive is receiving increasing concern. Herein, a simple and fast method for fluorescence detection of BPO is proposed based on consecutive chemical reactions. In this approach, BPO first oxidizes Fe2+ into Fe3+ and the resulting Fe3+ then induces the opening of the spirolactam ring of a new rhodamine derivative, N-methoxy rhodamine-6G spirolactam, switching on fluorescence of the detection system. More importantly, the fluorescence response of the reaction system to BPO is rather rapid and sensitive, with a detection limit of 6 mg kg−1 (k = 3), which makes it to be of great potential use in food safety analysis. The applicability of the proposed method has been successfully demonstrated on the determination of BPO in wheat flour samples.

  18. Comparison of the efficacy and safety of topical clindamycin and 5% benzoyl peroxide with nadifloxacin cream and 5% benzoyl peroxide gel in the treatment of acne vulgaris and assessment of the effects of these treatments on quality of life

    Directory of Open Access Journals (Sweden)

    Aslıhan Kırkağaç

    2015-03-01

    Full Text Available Background and Design: Acne vulgaris is a multifactorial chronic inflammatory disase of the pilosebaceous unit. Topical antibiotics and anti-inflammatory treatment are used for mild and moderate acne. Clindamycin is frequently used for acne treatment, altough nadifloxacin is a relatively new agent. There are few studies evaluating nadifloxacin efficacy. It's impact on quality of life has not been determined previously. In this study, it is aimed to compare the effect of these two agents, and to evaluate the effect of these treatments on quality of life. Materials and Methods: Eighty patients with mild-moderate acne vulgaris were divided in two groups of 40 people that had no difference in terms of age, gender and acne severity. The combination of topical clindamycin and 5% benzoyl peroxide gel twice a day was given to group 1 for 12 weeks. The combination of nadifloxacin cream and 5% benzoyl peroxide gel twice a day was given to group 2 for 12 weeks. The number of the inflammatory and non-inflammatory lesions were recorded at baseline and on weeks 2, 4, 8, 12 and side effects were recorded and evaluated. Global improvement was evaluated separately by patients and doctor after the treatment. Before and after the treatment, the quality of life of the patients were evaluated with Skindex-29. Results: Both treatment group regimens were significantly effective on inflammatory and non-inflammatory lesions and were well tolerated by patients in terms of side effects. It was also observed that there was statistically significant recovery after treatment in terms of clinical severity and quality of life. There was not any statistically significant difference between two treatment methods in terms of effectiveness, side effect and quality of life. Conclusion: Nadifloxacin and 5% benzoyl peroxide combination is effective in the treatment and improvement of quality of life in acne patients.

  19. Spectrophotometric speciation of Fe(II) and Fe(III) using hydrazone-micelle systems and flow injections

    International Nuclear Information System (INIS)

    Two hydrazones were synthesised, namely salicylhyrazone (SH) and trihydroxyacetophenone (THAPH) were synthesised with the objective of developing a method for determining of Fe(II) and Fe(III) in the presence of each other and hence the total iron.those hydrazones were selected so as to combine the ability of phenolic compounds to complex Fe(III) ions and the complexing characteristics of hydrazones. The complexes of Fe(II)SH and Fe(III)SH as well those of Fe(II)-THAPH and Fe(III)-THAPH had shown maximum absorbance at λ=412 nm which was not not modified by presence of micelles i.e. sodium n-dodecyl sulphate (SDS) and n-hexa dodecyl pyridinium bromide. The maximum absorbance for all complexes takes place around a neutral pH. Generally, in addition, of n-hexa dodecylpyridinium bromide to fe(II)-SH and Fe(III)-SH absorbance of the complexes increases with increasing the concentration of the micelle. The effects of the addition of sodium n-dodecyle sulphate (SDS) to Fe(III)-SH is also studied. Generally, increasing the concentration of the micelle decrease the absorbance of the complexes. To study the effect of the presence of Fe(II) and Fe(III) on the determination of each other,mixtures of Fe(II)-SH and Fe(III)-SH are studied. However, the use of ascorbic acid as a reducing reagent for Fe(III) did not produce the needed results but non reducible results, which may be due to the masking effect of ascorbic acid and thus making the metal not available to the ligand. However, conversion of Fe(II) to Fe(III) prior to the determination was avoided as this requires the use of oxidant, which will oxidise the ligand as well. To establish the condition for the maximum absorbance of THAPH complexes, the effect of the base was investigated by using sodium and ammonium hydroxide. Generally, increasing the concentration of the base decreases the abosrbance. as expected, ammonium hydroxide produced positive results than sodium hydroxide. After establishing the optimum Fi

  20. Synthesis, Characterization, and Biological Activity of Some Transition Metal Complexes of N-Benzoyl-N′-2-thiophenethiocarbohydrazide

    Directory of Open Access Journals (Sweden)

    Mahendra Yadav

    2012-01-01

    Full Text Available In the present study, Mn(II, Fe(II, Ni(II, and Cu(II complexes of N-benzoyl -N′-2-thiophenethiocarbohydrazide (H2 BTTH have been synthesized and characterized by elemental analysis, magnetic susceptibility measurements, infrared, NMR, electronic, and ESR spectral studies. The complexes were found to have compositions [Mn(H BTTH2], [Ni(BTTH(H2O2], [Cu(BTTH], and [Fe(H BTTH2EtOH]. The antibacterial and antifungal properties of H2 BTTH and its metal complexes have been screened against several bacteria and fungi.

  1. Extractive properties of benzohydroxamic and N-benzoyl-benzohydroxamic acids as analytical reagents towards six transition metal ions

    International Nuclear Information System (INIS)

    Two hydroxamic acids were prepared: benzohydroxamic and N-benzoyl benzohydroxamic acids. The former was prepared by coupling the free hydrox amine with benzoyl chloride with the ratio 1:1 in alkaline medium, where as the latter by the same procedure with the ratio 1:2 respectively, they were identified by their melting points, elemental analysis of their nitrogen contents. infra-red spectrophotometry, as well as their nitrogen using elevation of boiling point and the titration method to determine their molecular weights. The two hydroxamic acids were used as analytical reagents for the extraction of the metals Cr(vi), Fe(III), Ti(iv), Co(II) and U(vi). Benzohydroxamic acid has a maximum extraction 99.55% for Cr.(vi) 3M H2SO4, of 90.16% for Ti(iv) at pH 2.0,of 80.56% for Co(II) at pH 8.0 and 98.01% for U(vi) at pH 6.0. N-benzoyl benzohydroxamic acid has a maximum extraction of 96.45% for Cr(vi) at 3M H2So4, of 90.82% for Fe(III) at pH 4.0, of 97.02% for V(v) at 3M H2So4, of 83.56% for Ti(iv) at pH 2.0, of 89.82% for Co(II) at pH 8.0 and of 97.16% for U(vi) at pH 6.0. at the same pH of maximum extraction using heavy matrix, synthetic sea-water, benzohydroxamic acid has maximum values of 91.08%, of 77.99%, of 91.39%, of 87.50 and of 93.17% for Cr(vi), Fe(III), V(v), Ti(iv), Co9II) and U(vi) respectively whereas n-benzoyl benzohydroxamic acid has maximum values of 86.17%, of 77.78%, of 89.61%, of 75.66%, of 79.63% and of 91.18% for Cr(vi), Fe(III), V(v), Ti(iv), Co(II) and U(vi) respectively. The ratio of metal to ligand was determined utilizing the continuous variation method. It was 1 :2, 1: 1, 1 : 1, 1 : 2, 1: 2 and 1 : 2 with respect to Cr(vi), fe(III), Ti(iv), Co(II) and U(vi) respectively.(Author)

  2. Extraction of trace thorium from hydrochloric acid media by 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone

    Institute of Scientific and Technical Information of China (English)

    YANG Wei-Fan; YUAN Shuang-Gui; XU Yan-Bing; XIAO Yong-Hou; XIONG Bing

    2003-01-01

    The paper describes the solvent extraction of trace thorium from hydrochloric acid media by1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) using a radioactive tracer technique. The percent extraction ofthorium was studied as a function of acidity, PMBP concentration and equilibrium time. The back-extraction behaviorof thorium from the organic phase was also tested. Separation of thorium was performed from fission products pro-duced in 14 MeV neutron bombardment of natural uranium by employing the PMBP extraction procedure. Thegamma-ray spectra of the separated thorium fractions show that thorium can be separated from most of fission prod-ucts and a large amount of uranium.

  3. Evaluation of two forms of N-benzoyl-L-tyrosyl p-aminobenzoic acid in pancreatic function testing of dogs.

    Science.gov (United States)

    Burrows, C F; Orfely, C

    1989-01-01

    Plasma para-aminobenzoic acid (PABA) concentrations were compared in 12 dogs after oral administration of either a powdered suspension or a solution of N-benzoyl-L-tyrosyl-PABA. Peak PABA plasma concentrations were significantly higher at 30, 60 and 90 minutes after administration of the solution (P less than 0.05). As the solution may now be used as a clinical test, interpretation of the results by comparison with normal absorption curves obtained after administration of the suspension could contribute to a failure to diagnose canine exocrine pancreatic insufficiency. PMID:2784215

  4. Thermodynamic parameters for the extraction of some lanthanides with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 and trioctylamine

    International Nuclear Information System (INIS)

    The synergistic extraction of Pr, Gd and Yb with a mixture of 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 and trioctylamine diluted in C6H6, CHCl3 and CCl4 at 288 K, 298 K, 308 K and 318 K has been investigated. The values of the equilibrium constants as well as of ΔH0, ΔS0 and ΔG0 have been calculated. The thermodynamic parameters indicate that the adduct formed becomes stable on the account of the enthalpy change which exceeds the antistabilizing effect of the entropy factor. A comparison is made to the extraction of the same elements with thenoyltrifluoroacetone. (Author)

  5. Influence of the temperature on the extraction of some lanthanides with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5

    International Nuclear Information System (INIS)

    The extraction of Pr, Gd and Yb with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5(HPMBP) diluted in CHCl3, C6H6, and CCl4 at 288 K, 298 K, 308 K, and 318 K has been investigated. A compound of the type Me(PMBP)3HPMBP is formed in the organic phase. The values of the thermodynamic constants as well as of the parameters ΔH0, ΔS0 and ΔG0 have been determined. (Author)

  6. An efficient combination of Zr-MOF and microwave irradiation in catalytic Lewis acid Friedel-Crafts benzoylation.

    Science.gov (United States)

    Doan, Tan L H; Dao, Thong Q; Tran, Hai N; Tran, Phuong H; Le, Thach N

    2016-05-01

    A zirconium-based metal-organic framework, an effective heterogeneous catalyst, has been developed for the Friedel-Crafts benzoylation of aromatic compounds under microwave irradiation. Constructed by a Zr(iv) cluster and a linker 1,4-bis(2-[4-carboxyphenyl]ethynyl)benzene (H2CPEB), the MOF, possessing large pores and high chemical stability, was appropriate for the enhancement of Lewis acid activity under microwave irradiation. The reaction studies demonstrated that the material could give high yields for a few minutes and maintain its reactivity and structure over several cycles. PMID:27064371

  7. Antischistosomal activity of acridanone- hydrazones in Cebus monkeys experimentally infected with the SJ strain of Schistosoma mansoni

    Directory of Open Access Journals (Sweden)

    Paulo Marcos Zech Coelho

    1995-09-01

    Full Text Available In this study, four compounds were utilized at the dose of 12.5mg/kg body weight, p.o., to treat Cebus monkeys experimentally infected with about 200 cercariae of Schistosoma mansoni (SJ strain, via transcutaneous route. The oograms performed with rectal snips, as well as stool examinations carried out periodically, showed no viable eggs of the parasite, from day 29 to 226post-treatment. The perfusion undertaken after killing the animals showed absence of worms in the treated monkeys, whereas 83 worms were recovered from the control, thus corroborating the results obtained by means of oograms and coproscopy. These results confirm the efficacy of 9-acridanone- hydrazones previously tested against the LE strain of S. mansoni. The low curative dose and apparent absence of toxicity render these dmgs an important therapeutic reserve, taking into consideration the reports on the resistance of S. mansoni to the modern drugs oxamniquine and praziquantel.

  8. Cycloisomerization of acetylenic oximes and hydrazones under gold catalysis: Synthesis and cytotoxic evaluation of isoxazoles and pyrazoles

    Indian Academy of Sciences (India)

    J C Jeyaveeran; Chandrasekar Praveen; Y Arun; A A M Prince; P T Perumal

    2016-01-01

    The synthesis of substituted isoxazoles and pyrazoles through a general cycloisomerization methodology has been reported. The capability of gold(III) chloride to promote cycloisomerization of both , -acetylenic oximes and , -acetylenic hydrazones is the centrepiece of the strategy. A range of acetylenic precursors were investigated to afford 28 examples of the products with good to excellent chemical yields. Selected compounds were screened for their cytotoxic potential towards COLO320 cancer cell lines. The IC50 values of the tested compounds were in the micromolar range, with the best compound, 5-(6-Methoxy-naphthalen-2-yl)-3-phenyl-isoxazole (3h) displaying an IC50 of 38.9 M. For this compound, the crystal structure in complex with Aurora-A kinase was obtained which revealed details of its binding mode within the active site with a free energy of binding -9.54 kcal/mol.

  9. Semisynthesis and quantitative structure-activity relationship (QSAR) study of some cholesterol-based hydrazone derivatives as insecticidal agents.

    Science.gov (United States)

    Yang, Chun; Shao, Yonghua; Zhi, Xiaoyan; Huan, Qu; Yu, Xiang; Yao, Xiaojun; Xu, Hui

    2013-09-01

    In continuation of our program aimed at the discovery and development of natural-product-based insecticidal agents, four series of novel cholesterol-based hydrazone derivatives were synthesized, and their insecticidal activity was tested against the pre-third-instar larvae of oriental armyworm, Mythimna separata (Walker) in vivo at 1mg/mL. All the derivatives showed the better insecticidal activity than their precursor cholesterol. Quantitative structure-activity relationship (QSAR) model demonstrated that six descriptors such as RDF085v, Mor06u, Mor11u, Dv, HATS0v and H-046, are likely to influence the insecticidal activity of these compounds. Among them, two important ones are the Mor06u and RDF085v. PMID:23891182

  10. PET imaging of infection with a HYNIC-conjugated LTB4 antagonist labeled with F-18 via hydrazone formation

    Energy Technology Data Exchange (ETDEWEB)

    Rennen, Huub J.J.M. [Department of Nuclear Medicine, Radboud University Nijmegen Medical Centre, P.O. Box 9101, 6500 HB Nijmegen (Netherlands)], E-mail: h.rennen@nucmed.umcn.nl; Laverman, Peter; Eerd, Julliette E.M. van; Oyen, Wim J.G.; Corstens, Frans H.M.; Boerman, Otto C. [Department of Nuclear Medicine, Radboud University Nijmegen Medical Centre, P.O. Box 9101, 6500 HB Nijmegen (Netherlands)

    2007-08-15

    It was previously shown that the {sup 99m}Tc-labeled hydrazinonicotinamide (HYNIC)-conjugated LTB4 antagonist MB81 visualized infectious foci in rabbits adequately and within a few hours after injection. Here, the bivalent HYNIC-conjugated LTB4 antagonist MB67 (analog of MB81) was fluorinated with {sup 18}F via hydrazone formation and tested in vivo. Methods: MB67 was [{sup 18}F]-fluorinated via reaction of the [{sup 18}F]-fluorinated intermediate p-[{sup 18}F]-fluorobenzaldehyde ([{sup 18}F]FB) and the HYNIC moiety of MB67 via hydrazone formation. For comparison, MB67 was also labeled with {sup 99m}Tc. The biodistribution of {sup 18}F- and {sup 99m}Tc-labeled MB67 was investigated in rabbits with intramuscular infection. Results: [{sup 18}F]-MB67 was obtained at a maximum specific activity of 1200 GBq/mmol and proved to be stable in phosphate buffered saline (PBS) at 37{sup o}C for at least 4 h. PET images obtained with [{sup 18}F]-MB67 clearly delineated the abscess at 2 and 4 h pi. Counting of dissected tissues at 4 h pi revealed an abscess uptake of 0.073{+-}0.005 %ID/g, as compared to 0.160{+-}0.010 %ID/g for the {sup 99m}Tc-labeled analog. Abscess-to-muscle ratios were 23{+-}4 for [{sup 18}F]-MB67 and 35{+-}9 for [{sup 99m}Tc]-MB67. Conclusion: The present study showed the feasibility of a new [{sup 18}F]-labeling methodology and its application in the production of a new PET tracer for imaging of infection, [{sup 18}F]-MB67.

  11. On the roles of close shell interactions in the structure of acyl-substituted hydrazones: An experimental and theoretical approach.

    Science.gov (United States)

    Saeed, Aamer; Ifzan Arshad, M; Bolte, Michael; Fantoni, Adolfo C; Delgado Espinoza, Zuly Y; Erben, Mauricio F

    2016-03-15

    The 2-(phenyl-hydrazono)-succinic acid dimethyl ester compound was synthesized by reacting phenylhydrazine with dimethylacetylene dicarboxylate at room temperature and characterized by elemental analysis, infrared, Raman, (1)H and (13)C NMR spectroscopies and mass spectrometry. Its solid state structure was determined by X-ray diffraction methods. The X-ray structure determination corroborates that the molecule is present in the crystal as the hydrazone tautomer, probably favored by a strong intramolecular N-H···O=C hydrogen bond occurring between the carbonyl (-C=O) and the hydrazone -C=N-NH- groups. A substantial fragment of the molecular skeleton is planar due to an extended π-bonding delocalization. The topological analysis of the electron densities (Atom in Molecule, AIM) allows characterization of intramolecular N-H···O interaction, that can be classified as a resonant assisted hydrogen bond (RAHB). Moreover, the Natural Bond Orbital population analysis confirms that a strong hyperconjugative lpO1→σ*(N2-H) remote interaction between the C2=O1 and N2-H groups takes place. Periodic system electron density and topological analysis have been applied to characterize the intermolecular interactions in the crystal. Weak intermolecular interactions determine the crystal packing, and the prevalence of non-directional dispersive contributions are inferred on topological grounds. The IR spectrum of the crystalline compound was investigated by means of density functional theory calculations carried out with periodic boundary conditions on the crystal, showing excellent agreement between theory and the experiments. The vibrational assignment is complemented with the analysis of the Raman spectrum. PMID:26761413

  12. 香草醛水杨酰腙的合成%The Systhesis of Vanillin Salicylic Acyi Hydrazone

    Institute of Scientific and Technical Information of China (English)

    余锐; 王进; 曹国强; 付灿

    2014-01-01

    Salicylic hydrazide was preparation through methyl salicylate and 80%of hydrazine hydrate, vanillin salicylic acyl hydrazone was synthesized through salicylic hydrazide and vanilla aldehyde condensation reaction, with glacial acetic acid as catalyst, vanillin salicylic acyl hydrazone structures have been characterized by determining the melting point of the product and infrared spectrum. The effect of the heating reflux time, reaction temperature and reactant ratio on the yield was studied, its bacteriostatic activity of staphylococcus aureus were tested. Results show that the temperature is 65℃, time of heating reflux is 2h and raw material salicylic hydrazide and vanillin mole ratio is 1∶1.4, the yield can be as high as 73.4%.%以水杨酸甲酯与80%的水合肼为原料,制备水杨酰肼,然后以冰醋酸为催化剂,通过水杨酰肼与香草醛的缩合反应,合成了香草醛水杨酰腙。测定了产物的熔点,并用红外光谱对产物香草醛水杨酰腙的结构进行了表征。研究了反应温度、加热回流时间和反应物投料比对产率的影响,并测定其抑菌活性。结果表明:在温度65℃,加热回流时间2h和原料水杨酰肼与香草醛摩尔比为1∶1.4的条件下,产品产率高达73.4%。

  13. Thermal properties and DNA-binding studies of a new kind of acyl hydrazone compounds containing imidazole ring

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Jingwen; Liu, Xiangrong, E-mail: xkchemistry@163.com; Yang, Zaiwen; Zhao, Shunsheng

    2014-04-01

    Graphical abstract: - Highlights: • The single crystals of three new acyl hydrazone compounds are obtained and characterized. • The sequence of the thermostability studied by TG-DTG for three compounds under nitrogen and air is the same: III > I > II. • UV–Vis absorption shows the interaction modes of three compounds with CT-DNA are hyperchromic and hypochromic effects. • The results of three compounds reacting with CT-DNA gained by microcalorimeter show reactions are endothermic and rapid. - Abstract: Three new acyl hydrazone compounds C{sub 12}H{sub 12}N{sub 4}O{sub 3} (I), C{sub 12}H{sub 14}N{sub 4}O{sub 4} (II) and C{sub 16}H{sub 16}N{sub 4}O{sub 3} (III) are synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The crystal structural analyses show that the three compounds crystallize in the monoclinic crystal lattice. Their thermal decomposition processes under nitrogen and air are studied by TG-DTG, the sequence of the thermostability for three compounds at each condition is the same: III > I > II. The interaction modes of the three compounds with CT-DNA are investigated by UV–Vis absorption, showing hyperchromic and hypochromic effects. The thermogenic curves of the three compounds reacting with CT-DNA are measured by microcalorimetry, indicating that they are all endothermic reaction and the reaction times are within 10–30 min.

  14. 香草醛水杨酰腙的合成%The Systhesis of Vanillin Salicylic Acyi Hydrazone

    Institute of Scientific and Technical Information of China (English)

    余锐; 王进; 曹国强; 付灿

    2014-01-01

    以水杨酸甲酯与80%的水合肼为原料,制备水杨酰肼,然后以冰醋酸为催化剂,通过水杨酰肼与香草醛的缩合反应,合成了香草醛水杨酰腙。测定了产物的熔点,并用红外光谱对产物香草醛水杨酰腙的结构进行了表征。研究了反应温度、加热回流时间和反应物投料比对产率的影响,并测定其抑菌活性。结果表明:在温度65℃,加热回流时间2h和原料水杨酰肼与香草醛摩尔比为1∶1.4的条件下,产品产率高达73.4%。%Salicylic hydrazide was preparation through methyl salicylate and 80%of hydrazine hydrate, vanillin salicylic acyl hydrazone was synthesized through salicylic hydrazide and vanilla aldehyde condensation reaction, with glacial acetic acid as catalyst, vanillin salicylic acyl hydrazone structures have been characterized by determining the melting point of the product and infrared spectrum. The effect of the heating reflux time, reaction temperature and reactant ratio on the yield was studied, its bacteriostatic activity of staphylococcus aureus were tested. Results show that the temperature is 65℃, time of heating reflux is 2h and raw material salicylic hydrazide and vanillin mole ratio is 1∶1.4, the yield can be as high as 73.4%.

  15. Synthesis of novel flavone hydrazones: in-vitro evaluation of α-glucosidase inhibition, QSAR analysis and docking studies.

    Science.gov (United States)

    Imran, Syahrul; Taha, Muhammad; Ismail, Nor Hadiani; Kashif, Syed Muhammad; Rahim, Fazal; Jamil, Waqas; Hariono, Maywan; Yusuf, Muhammad; Wahab, Habibah

    2015-11-13

    Thirty derivatives of flavone hydrazone (5-34) had been synthesized through a five-step reaction and screened for their α-glucosidase inhibition activity. Chalcone 1 was synthesized through aldol condensation then subjected through oxidative cyclization, esterification, and condensation reaction to afford the final products. The result for baker's yeast α-glucosidase (EC 3.2.1.20) inhibition assay showed that all compounds are active with reference to the IC50 value of the acarbose (standard drug) except for compound 3. Increase in activity observed for compounds 2 to 34 clearly highlights the importance of flavone, hydrazide and hydrazone linkage in suppressing the activity of α-glucosidase. Additional functional group on N-benzylidene moiety further enhances the activity significantly. Compound 5 (15.4 ± 0.22 μM), a 2,4,6-trihydroxy substituted compound, is the most active compound in the series. Other compounds which were found to be active are those having chlorine, fluorine, and nitro substituents. Compounds with methoxy, pyridine, and methyl substituents are weakly active. Further studies showed that they are not active in inhibiting histone deacetylase activity and do not possess any cytotoxic properties. QSAR model was being developed to further identify the structural requirements contributing to the activity. Using Discovery Studio (DS) 2.5, various 2D descriptors were being used to develop the model. The QSAR model is able to predict the pIC50 and could be used as a prediction tool for compounds having the same skeletal framework. Molecular docking was done for all compounds using homology model of α-glucosidase to identify important binding modes responsible for inhibition activity. PMID:26491979

  16. Substitution Effects and Linear Free Energy Relationships During Reduction of 4- Benzoyl-n-(4-substituted Benzyl)pyridinium Cations

    Science.gov (United States)

    Leventis, Nicholas; Zhang, Guo-Hui; Rawashdeh, Abdel-Monem M.; Sotiriou-Leventis, Chariklia; Gray, Hugh R. (Technical Monitor)

    2003-01-01

    In analogy to 4-(para-substituted benzoyl)-N-methylpyridinium cations (1-X's), the title species (2-X's, -X = -OCH3, -CH3, -H, -Br, -COCH3, -NO2) undergo two reversible, well-separated (E(sub 1/2) greater than or equal to 650 mV) one-electron reductions. The effect of substitution on the reduction potentials of 2-X's is much weaker than the effect of the same substituents on 1-X's: the Hammett rho-values are 0.80 and 0.93 for the 1st- and 2nd-e reduction of 2-X's vs. 2.3 and 3.3 for the same reductions of 1-X's, respectively. Importantly, the nitro group of 2-NO2 undergoes reduction before the 2nd-e reduction of the 4-benzoylpyridinium system. These results suggest that the redox potentials of the 4-benzoylpyridinium system can be course-tuned via p-benzoyl substitution and fine-tuned via para-benzyl substitution. Introducing the recently derived substituent constant of the -NO2(sup)- group (sigma para-NO2(sup)- = -0.97) yields an excellent correlation for the 3rd-e reduction of 2- NO2 (corresponding to the reduction of the carbonyl group) with the 2nd-e reduction of the other 2-X's, and confirms the electron donating properties of -NO2(sup)-.

  17. Benzoyl chloride derivatization with liquid chromatography-mass spectrometry for targeted metabolomics of neurochemicals in biological samples.

    Science.gov (United States)

    Wong, Jenny-Marie T; Malec, Paige A; Mabrouk, Omar S; Ro, Jennifer; Dus, Monica; Kennedy, Robert T

    2016-05-13

    Widely targeted metabolomic assays are useful because they provide quantitative data on large groups of related compounds. We report a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method that utilizes benzoyl chloride labeling for 70 neurologically relevant compounds, including catecholamines, indoleamines, amino acids, polyamines, trace amines, antioxidants, energy compounds, and their metabolites. The method includes neurotransmitters and metabolites found in both vertebrates and insects. This method was applied to analyze microdialysate from rats, human cerebrospinal fluid, human serum, fly tissue homogenate, and fly hemolymph, demonstrating its broad versatility for multiple physiological contexts and model systems. Limits of detection for most assayed compounds were below 10nM, relative standard deviations were below 10%, and carryover was less than 5% for 70 compounds separated in 20min, with a total analysis time of 33min. This broadly applicable method provides robust monitoring of multiple analytes, utilizes small sample sizes, and can be applied to diverse matrices. The assay will be of value for evaluating normal physiological changes in metabolism in neurochemical systems. The results demonstrate the utility of benzoyl chloride labeling with HPLC-MS/MS for widely targeted metabolomics assays. PMID:27083258

  18. Synthesis and Biological Activity of Novel Amino Acid-(N'-Benzoyl Hydrazide and Amino Acid-(N'-Nicotinoyl Hydrazide Derivatives

    Directory of Open Access Journals (Sweden)

    Sherine N. Khattab

    2005-09-01

    Full Text Available The coupling reaction of benzoic acid and nicotinic acid hydrazides with N- protected L-amino acids including valine, leucine, phenylalanine, glutamic acid and tyrosine is reported. The target compounds, N-Boc-amino acid-(N`-benzoyl- and N- Boc-amino acid-(N`-nicotinoyl hydrazides 5a-5e and 6a-6e were prepared in very high yields and purity using N-[(dimethylamino-1H-1,2,3-triazolo[4,5-b]pyridin-1-yl- methylene]-N-methyl-methanaminium hexafluorophosphate N-oxide (HATU as coupling reagent. The antimicrobial activity of the Cu and Cd complexes of the designed compounds was tested. The products were deprotected affording the corresponding amino acid-(N`-benzoyl hydrazide hydrochloride salts (7a-7e and amino acid-(N`- nicotinoyl hydrazide hydrochloride salts (8a-8e. These compounds and their Cu and Cd complexes were also tested for their antimicrobial activity. Several compounds showed comparable activity to that of ampicillin against S. aureus and E. coli.

  19. Utility of positron annihilation lifetime technique for the assessment of spectroscopic data of some charge-transfer complexes derived from N-(1-Naphthyl)ethylenediamine dihydrochloride.

    Science.gov (United States)

    Refat, Moamen S; Adam, Abdel Majid A; Sharshar, T; Saad, Hosam A; Eldaroti, Hala H

    2014-03-25

    In this work, structural, thermal, morphological, pharmacological screening and positron annihilation lifetime measurements were performed on the interactions between a N-(1-Naphthyl)ethylenediamine dihydrochloride (NEDA·2HCl) donor and three types of acceptors to characterize these CT complexes. The three types of acceptors include π-acceptors (quinol and picric acid), σ-acceptors (iodine) and vacant orbital acceptors (tin(IV) tetrachloride and zinc chloride). The positron annihilation lifetime parameters were found to be dependent on the structure, electronic configuration, the power of acceptors and molecular weight of the CT complexes. The positron annihilation lifetime spectroscopy can be used as a probe for the formation of charge-transfer (CT) complexes. PMID:24291622

  20. Improved efficiency in organic light-emitting devices with tris-(8-hydroxyquinoline) aluminium doped 9,10-di(2-naphthyl) anthracene emission layer

    International Nuclear Information System (INIS)

    Organic light-emitting devices with tris-(8-hydroxyquinoline) aluminium (Alq3) doped 9,10-di(2-naphthyl) anthracene (ADN) as the emission layer (EML) have been fabricated. These devices exhibit efficient electroluminescence (EL) originated from the Alq3 as the mass ratio of Alq3 to ADN was varied from 1 to 50%. The devices with an optimal Alq3 mass ratio of 10 wt% showed a peak EL efficiency and an external quantum efficiency of 9.1 cd A-1 and 2.7% at a luminance of 1371 cd m-2, which is improved by a factor of 2.2 compared with 4.1 cd A-1 and 1.2% at a luminance of 3267 cd m-2 for conventional devices with the neat Alq3 as the EML.

  1. Chemical modification of silica gel with synthesized Schiff base hydrazone derivative and application for preconcentration and separation of U(VI) ions from aqueous solutions

    International Nuclear Information System (INIS)

    Schiff base hydrazone derivative (HL) sorbent was synthesized according to the literature to be used in the adsorption and preconcentration of U(VI) ions from aqueous solution and it was exposed to immobilization, and new solid support material was obtained. For this purpose, Schiff base hydrazone derivative (HL) was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane, then analyzed by Fourier transform infrared, Brunauer-Emmett-Teller, scanning electron microscopy and elemental analysis. The influence of the solution pH, amount of sorbent, contact time, temperature, foreign ion effect and initial U(VI) concentration was investigated. The maximum U(VI) uptake capacity was found to be 8.46 mg/g. (author)

  2. Randomized, Observer-blind, Split-face Compatibility Study with Clindamycin Phosphate 1.2%/Benzoyl Peroxide 3.75% gel and Facial Foundation Makeup

    Science.gov (United States)

    Pillai, Radhakrishnan

    2015-01-01

    Background: Cosmetic compatibility in the treatment of acne is an important issue significantly impacting quality of life, but often overlooked, as dermatologists commonly recommended avoidance of cosmetic foundations when treating adult female patients. Fixed combinations of clindamycin/benzoyl peroxide are widely used in the treatment of acne, but little is known about the impact of their concomitant use with facial foundation. Objective: To assess the compatibility of clindamycin phosphate 1. 2%/benzoyl peroxide 3. 75% gel with foundation makeup for up to six hours after application. Methods: Twenty-nine female subjects applied makeup to their face after randomly applying clindamycin phosphate 1. 2%/benzoyl peroxide 3. 75% gel to one side of the face. Investigator and subject self- assessment included facial skin attributes, facial tolerability, and cosmetic compatibility post-application and at Hour 6; as well as cutaneous tolerability. Results: No statistical difference was noted between the treated and untreated side of the face in terms of coverage, blotchiness, appearance, skin tone, or visual smoothness. Tolerability was excellent, with no erythema, edema, dryness, and peeling post-makeup application. For both the treated and untreated side, there was a slight lack of improvement in cosmetic appearance six hours post-makeup application. Conclusion: Clindamycin/benzoyl peroxide 3. 75% gel was shown to have excellent cosmetic compatibility with facial foundation. PMID:26430488

  3. Synergistic extraction of uranyl and plutonyl ions with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP) and some some aliphatic sulphoxides

    International Nuclear Information System (INIS)

    Extraction of uranyl and plutonyl ions with 1-phenyl-3-methyl-4-benzoyl pyrazolone-5 (HPMBP) and some long chain aliphatic sulphoxides has been studied and the equilibrium constants for the organic phase addition reaction have been determined for both the systems. (author). 8 refs

  4. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    The retention indices of aliphatic alcohols of carbon number up to Cg, and of their benzoyl derivatives up to C7, were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH2- group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices Δl , and positional and structural increments δI, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs

  5. Benzoylation of Ergosterol through Nucleophilic Acyl Substitution and Subsequent Formation of Ergosterol Benzoate Endoperoxide by Reaction with Singlet Oxygen Generated by Photosensitization

    Science.gov (United States)

    Roslaniec, Mary C.; Sanford, Elizabeth M.

    2011-01-01

    Reactive oxygen species such as singlet oxygen have been a major focus of research in medicine. The effect of singlet oxygen on sterols within biological membranes is becoming increasingly more important. Ergosterol, a vitamin D precursor, is one such sterol. The benzoylation of ergosterol and subsequent reaction with singlet oxygen to form an…

  6. Structural and vibrational study of 8-hydroxyquinoline-2-carboxaldehyde isonicotinoyl hydrazone - A potential metal-protein attenuating compound (MPAC) for the treatment of Alzheimer's disease

    Science.gov (United States)

    de Freitas, Leonardo Viana; da Silva, Cecilia C. P.; Ellena, Javier; Costa, Luiz Antônio Sodré; Rey, Nicolás A.

    2013-12-01

    A comprehensive structural and vibrational study of the potential metal-protein attenuating compound 8-hydroxyquinoline-2-carboxaldehyde isonicotinoyl hydrazone is reported. X-ray diffraction data, as well as FT-IR and Raman frequencies, were compared with the respective theoretical values obtained from DFT calculations. Theory agrees well with experiment. In this context, an attempt of total assignment concerning the FT-IR and Raman spectra of the title compound was performed, shedding new light on previous partial assignments published elsewhere.

  7. An Eco-Friendly Ultrasound-Assisted Synthesis of Novel Fluorinated Pyridinium Salts-Based Hydrazones and Antimicrobial and Antitumor Screening

    OpenAIRE

    Nadjet Rezki; Salsabeel A. Al-Sodies; Mohamed R. Aouad; Sanaa Bardaweel; Mouslim Messali; El Ashry, El Sayed H.

    2016-01-01

    The present work reports an efficient synthesis of fluorinated pyridinium salts-based hydrazones under both conventional and eco-friendly ultrasound procedures. The synthetic approach first involves the preparation of halogenated pyridinium salts through the condensation of isonicotinic acid hydrazide (1) with p-fluorobenzaldehyde (2) followed by the nucleophilic alkylation of the resulting N-(4-fluorobenzylidene)isonicotinohydrazide (3) with a different alkyl iodide. The iodide counteranion ...

  8. A CuAAC-Hydrazone-CuAAC Trifunctional Scaffold for the Solid-Phase Synthesis of Trimodal Compounds: Possibilities and Limitations

    Czech Academy of Sciences Publication Activity Database

    Fabre, Benjamin; Pícha, Jan; Vaněk, Václav; Buděšínský, Miloš; Jiráček, Jiří

    2015-01-01

    Roč. 20, č. 10 (2015), s. 19310-19329. ISSN 1420-3049 R&D Projects: GA ČR GA14-17305S Institutional support: RVO:61388963 Keywords : click chemistry * multifunctional scaffold * solid-phase synthesis * protein mimics * copper * hydrazone * hydrazide Subject RIV: CC - Organic Chemistry Impact factor: 2.416, year: 2014 http://www.mdpi.com/1420-3049/20/10/19310/htm

  9. X-ray and DFT calculated structures of 2-(1 H-imidazol-1-yl)-1-(2-naphthyl)ethan-1-one N-phenylthiosemicarbazone and 2-(1 H-imidazol-1-yl)-1-(2-naphthyl)ethan-1-one N-(4-chlorophenyl)thiosemicarbazone

    Science.gov (United States)

    Sahin, Z. S.; Septioglu, E.; Calis, U.; Isik, S.

    2014-12-01

    Crystal and molecular structures of two new compounds 2-(1 H-imidazol-1-yl)-1-(2-naphthyl)ethan-1-one N-phenylthiosemicarbazone, C22H19N5S, ( I) and 2-(1 H-imidazol-1-yl)-1-(2-naphthyl)ethan-1-one N-(4-chlorophenyl)thiosemicarbazone, C22H18ClN5S, ( II) have been determined by single-crystal X-ray diffraction. Molecular geometries from X-ray experiment of I and II have been compared with those calculated using the Density Functional Theory (DFT) with B3LYP/6-31G( d, p) basis set. Both compounds crystallize in the monoclinic space group P21/ c with Z = 4: a = 13.2880(5), 14.2648(3) Å, b = 9.4122(2), 9.3892(3) Å, c = 15.6341(6), 15.6268(4) Å, β = 101.779(3)°, 104.926(2)°, for I and II, respectively. An extensive two-dimensional network of N-H⋯N hydrogen bonds and π-ring interactions are responsible for crystal stabilization in both structures.

  10. COMPARATIVE STUDY OF CLINICAL EFFICACY AND SIDE EFFECTS OF ADAPALENE 0.1% GEL AND BENZOYL PEROXIDE 2.5% GEL AS MONOTHERAPIES AND COMBINATION THERAPY IN FACIAL ACNE: INDIAN PERSPECTIVE

    Directory of Open Access Journals (Sweden)

    Adarsh

    2014-04-01

    Full Text Available A fixed dose combination gel with adapalene 0.1% and benzoyl peroxide 2.5% has been developed for the once daily treatment of acne vulgaris .This fixed combination was approved by U.S FDA in December 2008. This study was done in the Department of Dermatology, KIMS, Bangalore to assess the efficacy and adverse effects of topical adapalene 0.1%–benzoyl peroxide 2.5% combination gel as compared to topical adapalene 0.1% gel and 2.5% benzoyl peroxide gel (monotherapies in the treatment of facial acne vulgaris. To the best of our knowledge, this is one of the few studies conducted in India. It was an open label study. Participants received either adapalene 0.1% gel, benzoyl peroxide 2.5% gel or adapalene 0.1% – benzoyl peroxide 2.5% combination gel for 12 weeks. Follow up was done at the end of 1,2,4,8 and 12 weeks. Evaluation included lesion count and adverse events. Participants included males and females aged between 18-38 years with grade 2 or 3 facial acne vulgaris as per investigators global assessment of acne scale. A total of 62 participants were recruited out of which 23 were males and 39 were females.88.71% participants completed the study. The study revealed that combination of adapalene 0.1% and benzoyl peroxide 2.5% gel was more effective in the treatment of facial acne as compared to adapalene 0.1% gel and benzoyl peroxide 2.5% gel (topical monotherapies. The safety of combination of adapalene 0.1% and benzoyl peroxide 2.5% gel was comparable with adapalene 0.1% gel and benzoyl peroxide 2.5% gel monotherapies.

  11. Effect of temperature and concentration on benzoyl peroxide bleaching efficacy and benzoic acid levels in whey protein concentrate.

    Science.gov (United States)

    Smith, T J; Gerard, P D; Drake, M A

    2015-11-01

    Much of the fluid whey produced in the United States is a by-product of Cheddar cheese manufacture and must be bleached. Benzoyl peroxide (BP) is currently 1 of only 2 legal chemical bleaching agents for fluid whey in the United States, but benzoic acid is an unavoidable by-product of BP bleaching. Benzoyl peroxide is typically a powder, but new liquid BP dispersions are available. A greater understanding of the bleaching characteristics of BP is necessary. The objective of the study was to compare norbixin destruction, residual benzoic acid, and flavor differences between liquid whey and 80% whey protein concentrates (WPC80) bleached at different temperatures with 2 different benzoyl peroxides (soluble and insoluble). Two experiments were conducted in this study. For experiment 1, 3 factors (temperature, bleach type, bleach concentration) were evaluated for norbixin destruction using a response surface model-central composite design in liquid whey. For experiment 2, norbixin concentration, residual benzoic acid, and flavor differences were explored in WPC80 from whey bleached by the 2 commercially available BP (soluble and insoluble) at 5 mg/kg. In liquid whey, soluble BP bleached more norbixin than insoluble BP, especially at lower concentrations (5 and 10 mg/kg) at both cold (4°C) and hot (50°C) temperatures. The WPC80 from liquid whey bleached with BP at 50°C had lower norbixin concentration, benzoic acid levels, cardboard flavor, and aldehyde levels than WPC80 from liquid whey bleached with BP at 4°C. Regardless of temperature, soluble BP destroyed more norbixin at lower concentrations than insoluble BP. The WPC80 from soluble-BP-bleached wheys had lower cardboard flavor and lower aldehyde levels than WPC80 from insoluble-BP-bleached whey. This study suggests that new, soluble (liquid) BP can be used at lower concentrations than insoluble BP to achieve equivalent bleaching and that less residual benzoic acid remains in WPC80 powder from liquid whey

  12. Contribution to the study of the chemical effects of the (n, γ) reaction on copper N-benzoyl N-phenyl hydroxylaminate and copper N-benzoyl N-(o) Tolyl hydroxylaminate

    International Nuclear Information System (INIS)

    The influence of some factors such as pre-heating and pre-irradiation with gamma rays on the retention and thermal annealing of copper N-benzoyl N-phenyl hydroxylaminate and of copper N-benzolyl N-(o) tolyl hydroxylaminate is studied. The complexes were synthesized and characterized by determination of the melting-point, elemental analysis, X-ray diffraction, infra-red and visible range absoption spectrometry-thermogravimetric analysis were examined and the stability of the compounds was checked against heating and gamma irradiation from a 60Co source. Some experiments using the Szilard-Chalmers effect were carried out by irradiating the compound in the IEA-R1 nuclear reactor and calculating its specific activities. (M.J.C.)

  13. Simple and fast fluorescence detection of benzoyl peroxide in wheat flour by N-methoxy rhodamine-6G spirolactam based on consecutive chemical reactions

    Energy Technology Data Exchange (ETDEWEB)

    Chen Wei; Shi Wen; Li Zhao [Beijing National Laboratory for Molecular Sciences, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Ma Huimin, E-mail: mahm@iccas.ac.cn [Beijing National Laboratory for Molecular Sciences, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Liu Yang; Zhang Jinghua; Liu Qingjun [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2011-12-05

    Graphical abstract: A simple and fast method for fluorescence detection of benzoyl peroxide in wheat flour by N-methoxy rhodamine-6G spirolactam (1) is proposed based on consecutive chemical reactions. Highlights: Black-Right-Pointing-Pointer Benzoyl peroxide can oxidize Fe{sup 2+} into Fe{sup 3+}. Black-Right-Pointing-Pointer Fe{sup 3+} selectively induces the opening of rhodamine spirolactam ring. Black-Right-Pointing-Pointer The two reactions led to the development of a new fluorescent method for benzoyl peroxide. Black-Right-Pointing-Pointer The method is simple and fast, and is used to detect benzoyl peroxide in wheat flour. - Abstract: Benzoyl peroxide (BPO) as a brightener is often added to wheat flour, and excessive use of this food additive is receiving increasing concern. Herein, a simple and fast method for fluorescence detection of BPO is proposed based on consecutive chemical reactions. In this approach, BPO first oxidizes Fe{sup 2+} into Fe{sup 3+} and the resulting Fe{sup 3+} then induces the opening of the spirolactam ring of a new rhodamine derivative, N-methoxy rhodamine-6G spirolactam, switching on fluorescence of the detection system. More importantly, the fluorescence response of the reaction system to BPO is rather rapid and sensitive, with a detection limit of 6 mg kg{sup -1} (k = 3), which makes it to be of great potential use in food safety analysis. The applicability of the proposed method has been successfully demonstrated on the determination of BPO in wheat flour samples.

  14. Extraction of lanthanide by 4-benzoyl-3-methyl-1-phenylpyrazol-5-one (HPMBP) in ionic liquid medium

    International Nuclear Information System (INIS)

    Solvent extraction of Lu by a beta diketone, 4-benzoyl-3-methyl-1- phenylpyrazol-5-one (HPMBP) in a RTIL, 1- methyl-3-octylimidazolium bis(trifluoromethylsulphonyl) imide, (C8mimNTf2) was studied as a function of aqueous acidity, and ligand concentration. The distribution ratio (D) of Lu decreased with increasing acidity. Metal-ligand stoichiometry was arrived at 1:3 by slope method of log-log plot. Similarly the dependence on H+ ion was also shown to be three. With this information, the extraction mechanism was proposed to be of typical of these type of acidic extractants, i.e. cation-exchange, which was not typical with this extractant dissolved in butyl analogue of above RTIL. (author)

  15. Propene Polymerisation with rac-[Me2Si(2-Me-4-(Naphthyl)-1-Ind)2]ZrCl2 as a Highly Active Catalyst: Influence of Monomer Concentration, Polymerisation Temperature and a Heterogenising Support

    OpenAIRE

    M.Frediani; Kaminsky, W.

    2003-01-01

    Propene was polymerised at high temperatures (up to 90 °C) using rac-[Me2Si(2-Me-4-(α-naphthyl)-1-Ind)2]ZrCl2/MAO as the catalytic system. The increasing deactivation reaction rate of the catalyst for polymerisations above 60 °C was less for a silica supported catalyst compared with the homogeneous one. The isotacticity of polypropene decreases from 99 to 96%. Also the morphology changes with different temperatures.

  16. Selective spectrophotometric determination of molybdenum(VI) and vanadium(V) with resacetophenone benzoic hydrazone in steels and alloys

    International Nuclear Information System (INIS)

    A spectrophotometric method for the determination of molybdenum(VI) and vanadium(V) using 2, 4-dihydroxyacetophenone benzoic hydrazone (RPBH) is reported. The reagent forms 1:1 yellow coloured complexes with Mo(VI) and V(V) at pH 3.5. The colour development of molybdenum complex is instantaneous and shows absorption maximum at 410nm. In the case of vanadium complex, maximum colour is developed after heating for 10 minutes on a water bath and show maximum absorption at 380nm. The molybdenum(VI) complex with a molar absorptivity of 3.6x103 l mol-1 cm-1 and Sandell's sensitivity of 0.02 μg/cm2, obeys Beer's law in the range 2.4 to 33.6 ppm. The vanadium(V) complex whose molar absorptivity and Sandell's sensitivity are 1.3x104 l mol-1 cm-1 and 0.004 μg/cm2 respectively, obeys Beer's law in the range 0.25 to 7.6 ppm. The effect of various diverse ions on the determination of the metal ions is studied. The method is applied for the determination of molybdenum and vanadium in steel and alloy samples. (author). 10 refs., 1 fig., 3 tabs

  17. Thermodynamics of substituted hydrazone and its Fe3+, UO22+, Cu2+ and Zn2+ complexes. Potentiometric and voltammetric studies

    International Nuclear Information System (INIS)

    Complex equilibria of o-hydroxyacetophenone isobutyroyl hydrazone (H2AIBuH) with proton and Fe3+, UO22+, Cu2+ and Zn2+ have been investigated potentiometrically in 0.1 M KCl and 20% (v/v)ethanol-water media. The order of stability constants has been found to be Fe3+ > UO22+ > Cu2+ > Zn2+. The dissociation of H2AIBuH and the stability constants of its Cu2+ complexes have been found to increase with decreasing ionic strength of the medium and increasing organic content of the aquo-organic solvent. The Gibbs free enthalpy of transfer from water to ethanol-water solvents was found to be positive and increases with increasing ethanol content. The formation of the metal complexes has been found to be spontaneous, exothermic and entropically favoured as indicated from the derived thermodynamic functions (ΔG, ΔH, ΔS). Polarographic and cyclic voltammetric behaviours of H2AIBuH have been investigated in Britton-Robinson buffers of pH 2-12. The mechanism of the reaction process has been postulated. Moreover, the kinetic and the thermodynamic parameters for the electrode process have been evaluated. (orig.)

  18. Growth and characterization of benzaldehyde 4-nitro phenyl hydrazone (BPH) single crystal: A proficient second order nonlinear optical material

    Science.gov (United States)

    Saravanan, M.; Abraham Rajasekar, S.

    2016-04-01

    The crystals (benzaldehyde 4-nitro phenyl hydrazone (BPH)) appropriate for NLO appliance were grown by the slow cooling method. The solubility and metastable zone width measurement of BPH specimen was studied. The material crystallizes in the monoclinic crystal system with noncentrosymmetric space group of Cc. The optical precision in the whole visible region was found to be excellent for non-linear optical claim. Excellence of the grown crystal is ascertained by the HRXRD and etching studies. Laser Damage Threshold and Photoluminescence studies designate that the grown crystal contains less imperfection. The mechanical behaviour of BPH sample at different temperatures was investigated to determine the hardness stability of the grown specimen. The piezoelectric temperament and the relative Second Harmonic Generation (for diverse particle sizes) of the material were also studied. The dielectric studies were executed at varied temperatures and frequencies to investigate the electrical properties. Photoconductivity measurement enumerates consummate of inducing dipoles due to strong incident radiation and also divulge the nonlinear behaviour of the material. The third order nonlinear optical properties of BPH crystals were deliberate by Z-scan method.

  19. A New, Once-daily, Optimized, Fixed Combination of Clindamycin Phosphate 1.2% and Low-concentration Benzoyl Peroxide 2.5% Gel for the Treatment of Moderate-to-Severe Acne

    OpenAIRE

    Gold, Michael H.

    2009-01-01

    The treatment of acne with combination therapy is commonplace with treatment aimed at sustained efficacy with minimal side effects, maximum adherence, and the avoidance of bacterial resistance. Combinations containing clindamycin and benzoyl peroxide have been shown to be effective, but the irritation caused by the concentration of benzoyl peroxide 5% in the more commonly used, fixed combinations can be limiting. In addition, surfactants, preservatives, and high levels of organic solvents, in...

  20. Enhanced hydrogenation activity and diastereomeric interactions of methyl pyruvate co-adsorbed with R-1-(1-naphthyl)ethylamine on Pd(111).

    Science.gov (United States)

    Mahapatra, Mausumi; Burkholder, Luke; Garvey, Michael; Bai, Yun; Saldin, Dilano K; Tysoe, Wilfred T

    2016-01-01

    Unmodified racemic sites on heterogeneous chiral catalysts reduce their overall enantioselectivity, but this effect is mitigated in the Orito reaction (methyl pyruvate (MP) hydrogenation to methyl lactate) by an increased hydrogenation reactivity. Here, this effect is explored on a R-1-(1-naphthyl)ethylamine (NEA)-modified Pd(111) model catalyst where temperature-programmed desorption experiments reveal that NEA accelerates the rates of both MP hydrogenation and H/D exchange. NEA+MP docking complexes are imaged using scanning tunnelling microscopy supplemented by density functional theory calculations to allow the most stable docking complexes to be identified. The results show that diastereomeric interactions between NEA and MP occur predominantly by binding of the C=C of the enol tautomer of MP to the surface, while simultaneously optimizing C=O····H2N hydrogen-bonding interactions. The combination of chiral-NEA driven diastereomeric docking with a tautomeric preference enhances the hydrogenation activity since C=C bonds hydrogenate more easily than C=O bonds thus providing a rationale for the catalytic observations. PMID:27488075

  1. Evaluation of structure-reactivity descriptors and biological activity spectra of 4-(6-methoxy-2-naphthyl)-2-butanone using spectroscopic techniques.

    Science.gov (United States)

    Agrawal, Megha; Deval, Vipin; Gupta, Archana; Sangala, Bagvanth Reddy; Prabhu, S S

    2016-10-01

    The structure and several spectroscopic features along with reactivity parameters of the compound 4-(6-methoxy-2-naphthyl)-2-butanone (Nabumetone) have been studied using experimental techniques and tools derived from quantum chemical calculations. Structure optimization is followed by force field calculations based on density functional theory (DFT) at the B3LYP/6-311++G(d,p) level of theory. The vibrational spectra have been interpreted with the aid of normal coordinate analysis. UV-visible spectrum and the effect of solvent have been discussed. The electronic properties such as HOMO and LUMO energies have been determined by TD-DFT approach. In order to understand various aspects of pharmacological sciences several new chemical reactivity descriptors - chemical potential, global hardness and electrophilicity have been evaluated. Local reactivity descriptors - Fukui functions and local softnesses have also been calculated to find out the reactive sites within molecule. Aqueous solubility and lipophilicity have been calculated which are crucial for estimating transport properties of organic molecules in drug development. Estimation of biological effects, toxic/side effects has been made on the basis of prediction of activity spectra for substances (PASS) prediction results and their analysis by Pharma Expert software. Using the THz-TDS technique, the frequency-dependent absorptions of NBM have been measured in the frequency range up to 3THz. PMID:27284764

  2. Photocatalytic H2 evolution from NADH with carbon quantum dots/Pt and 2-phenyl-4-(1-naphthyl)quinolinium ion.

    Science.gov (United States)

    Wu, Wenting; Zhan, Liying; Ohkubo, Kei; Yamada, Yusuke; Wu, Mingbo; Fukuzumi, Shunichi

    2015-11-01

    Carbon quantum dots (CQDs) were simply blended with platinum salts (K2PtCl4 and K2PtCl6) and converted into a hydrogen-evolution co-catalyst in situ, wherein Pt salts were dispersed on the surface of CQDs under photoirradiation of an aqueous solution of NADH (an electron and proton source) and 2-phenyl-4-(1-naphthyl)quinolinium ion (QuPh(+)-NA) employed as an organic photocatalyst. The co-catalyst (CQDs/Pt) exhibits similar catalytic reactivity in H2 evolution as that of pure Pt nanoparticles (PtNPs) although the Pt amount of CQDs/Pt was only 1/200 that of PtNPs previously reported. CQDs were able to capture the Pt salt acting as Pt supports. Meanwhile, CQDs act as electron reservoir, playing an important role to enhance electron transfer from QuPh(+)-NA to the Pt salt, which was confirmed by kinetic studies, XPS and HRTEM. PMID:25498411

  3. Crystal and Molecular Structure Studies of Ethyl 4-(4-Hydroxyphenyl-6-(6-methoxy-2-naphthyl-2-oxocyclohex-3-ene-1-carboxylate and Ethyl 4-(3-Bromophenyl-6-(6-methoxy-2-naphthyl-2-oxocyclohex-3-ene-1-carboxylate

    Directory of Open Access Journals (Sweden)

    Badiadka Narayana

    2012-08-01

    Full Text Available The crystal and molecular structures of the title compounds, ethyl 4-(4-hydroxyphenyl-6-(6-methoxy-2-naphthyl-2-oxocyclohex-3-ene-1-carboxylate (I and ethyl 4-(3-bromophenyl-6-(6-methoxy-2-naphthyl-2-oxocyclohex-3-ene-1-carboxylate (II, are reported and confirmed by single crystal X-ray diffraction data. Compound (I, C26H24O5, crystallizes from a methanol solution in the monoclinic C2/c space group with eight molecules in the unit cell. The unit cell parameters are: a = 25.4114(5 Å, b = 8.47440(10 Å, c = 20.6921(4 Å, β = 108.328(2° and V = 4229.92(13 Å3. Disorder is observed throughout the entire molecule with an occupancy ratio 0.690(2:0.310(2. Compound (II, C26H23O4Br, crystallizes from an ethyl acetate solution in the monoclinic P21/c spacegroup with four molecules in the unit cell. The unit cell parameters are a = 17.8991(9 Å, b = 11.4369(6 Å, c = 10.8507(5 Å, β = 92.428(4° and V = 2219.25(19 Å3. Disorder is observed in the cyclohexenone ring and the carboxylate group with an occupancy ratio 0.830(6:0.170(6. Weak O–H...O (I or C–H...O (II intermolecular interactions are observed which influence crystal packing stability. These chalcone derivative types of molecules are important in their ability to act as activated unsaturated systems in conjugated addition reactions of carbanions in the presence of basic catalysts which exhibit a multitude of biological activities.

  4. Synthesis, characterization and biological evaluation of N-ferrocenylmethyl amino acid benzene carboxamide derivatives and N-ferrocenyl benzoyl amino alkane derivatives as anti-cancer agents.

    OpenAIRE

    Butler, William E.

    2012-01-01

    The aim of this research was to explore the structure-activity relationship (SAR) of ferrocenyl-bioconjugates. A series of N-(ferrocenylmethylamino acid)-fluorinated-benzene carboxamide derivatives and a series of N-(ferrocenyl)-benzoyl-aminoalkane derivatives have been synthesised, structurally characterised and biologically evaluated for their anti-proliferative activity on various cancer cell lines, principally, the (estrogen receptor positive) MCF-7 breast cancer cell line. The anti-c...

  5. Investigating The Molecular Formation Ppoperties of 2-Acetylamino-6-Benzoyl-4-Chlorophenol Using The Semi Emprical Molecular Orbital Methods (PM3, AM1, MNDO)

    OpenAIRE

    Fatma BAYSEN

    2004-01-01

    In this study in order to the geometry optimization of the 2-acetylamino-6-benzoyl-4-chlorophenol crystal, which is used for forming analgesic and antienflamatuar medicine and of which crystal structure was determined using x-ray diffraction method, PM3, AM1 and MNDO semi emprical molecular orbital methods found in the HyperChem program were used. By the geometry optimization geometric parameters of the molecules having the minimum energy were found.These values which were theoretically obtai...

  6. Palladium(ii)-catalyzed C-C and C-O bond formation for the synthesis of C1-benzoyl isoquinolines from isoquinoline N-oxides and nitroalkenes.

    Science.gov (United States)

    Li, Jiu-Ling; Li, Wei-Ze; Wang, Ying-Chun; Ren, Qiu; Wang, Heng-Shan; Pan, Ying-Ming

    2016-08-01

    C1-Benzoyl isoquinolines can be generated via a palladium(ii)-catalyzed C-C and C-O coupling of isoquinoline N-oxides with aromatic nitroalkenes. The reaction proceeds through remote C-H bond activation and subsequent intramolecular oxygen atom transfer (OAT). In this reaction, the N-O bond was designed as a directing group in the C-H bond activation as well as the source of an oxygen atom. PMID:27443150

  7. SYNTHESIS AND EVALUATION OF ANTIMICROBIAL ACTIVITY OF 1-BENZOYL-1H-PYRAZOLO [4,3-C]QUINOLIN-4(5H-ONES

    Directory of Open Access Journals (Sweden)

    Shivashankar Murugesh

    2011-01-01

    Full Text Available A series of 1-benzoyl-1H-pyrazolo [4,3-C]quinolin-4(5H-one, carrying appropriate substituents at the Quinoline ring have been synthesized in good yields via the condensation of 4-chloro-3-formylquinolin-2[1H]ones with benzohydrazide using triethylamine as a base. All the synthesized compounds were evaluated for their antibacterial activities.

  8. Inactivation of Escherichia coli glycerol kinase by 5'-[p-(fluorosulfonyl)benzoyl]adenosine: protection by the hydrolyzed reagent

    International Nuclear Information System (INIS)

    Incubation of Escherichia coli glycerol kinase with 5'-[p-(fluorosulfonyl)benzoyl]adenosine (FSO2BzAdo) at pH 8.0 and 250C results in the loss of enzyme activity, which is not restored by the addition of β-mercaptoethanol or dithiothreitol. The FSO2BzAdo concentration dependence of the inactivation kinetics is described by a mechanism that includes the equilibrium binding of the reagent to the enzyme prior to a first-order inactivation reaction in addition to effects of reagent hydrolysis. The hydrolysis of the reagent has two effects on the observed kinetics. The first effect is deviation from pseudo-first-order kinetic behavior due to depletion of the reagent. The second effect is the novel protection of the enzyme from inactivation due to binding of the sulfonate hydrolysis product. Determinations of the reaction stoichiometry with 3H-labeled FSO2BzAdo show that the inactivation is associated with the covalent incorporation of 1.08 mol of reagent/mol of enzyme subunit. Ligand protection experiments show that ATP, AMP, dAMP, NADH, 5'-adenylyl imidodiphosphate, and the sulfonate hydrolysis product of FSO2BzAdo provide protection from inactivation. The protection obtained with ATMP is not dependent on Mg2+. The results are consistent with modification by FSO2BzAdo of a single adenine nucleotide binding site per enzyme subunit

  9. Topical therapy for acne in women: is there a role for clindamycin phosphate-benzoyl peroxide gel?

    Science.gov (United States)

    Del Rosso, James Q

    2014-10-01

    Acne vulgaris (AV) in adult women is commonly encountered in clinical dermatology practice. This patient subset often experiences psychosocial effects that differ in some ways from those experienced by adolescent females with AV, as they were not expecting to have to deal with this disorder beyond their adolescent years. Most of the emphasis on therapy for adult women with AV has focused on use of oral contraceptives (OCs) and/or oral spironolactone, with little to no evaluation or discussion of topical agents in this patient group. This article provides an overview of AV in adult women and presents the results of a subanalysis of data from female patients who were treated in phase 3 studies with clindamycin phosphate (CP) 1.2%-benzoyl peroxide (BP) 2.5% gel once daily for facial AV. The subanalysis compared outcomes in females younger than 25 years and in those 25 years and older. Overall, the data showed that therapeutic outcomes were comparable between the 2 groups. PMID:25372252

  10. Metabolic fate of N-benzoyl-N'-phenyl-2,6-diaminobenzoic acid in rats and guinea pigs

    International Nuclear Information System (INIS)

    The metabolism of N-benzoyl-N'-phenyl-2, 6-diaminobenzoic acid (F-1) was studied by a radiotracer technique. When 14C-F-1 was administered to rats and guinea pigs, benzoic acid, p-hydroxybenzoic acid, and glycine conjugates of these compounds were found in the urine as its metabolites. In the case of 3H-F-1 administration, it was possible to detect N-acetyl-N'-phenyl-2, 6-diaminobenzoic acid in the urine as a major metabolite. Rats and guinea pigs excreted in the feces a majority of radioactivity as unchanged F-1. The uptake of 3H-activity into the CMC pouch was considerably higher 12 hours after the oral administration of 3H-F-1 to inflamed rats. A large amount of unchanged F-1 rather than N-acetyl-N'-phenyl-2, 6-diaminobenzoic acid (metabolite 1) was found in the CMC pouch. On the other hand, in the liver the amount of metabolite 1 was larger than the unchanged parent compound F-1. These facts were taken into account in an attempt to determine the mode of action of the anti-inflammatory effect of F-1. (auth.)

  11. Characterization of some amino acid derivatives of benzoyl isothiocyanate: Crystal structures and theoretical prediction of their reactivity

    Science.gov (United States)

    Odame, Felix; Hosten, Eric C.; Betz, Richard; Lobb, Kevin; Tshentu, Zenixole R.

    2015-11-01

    The reaction of benzoyl isothiocyanate with L-serine, L-proline, D-methionine and L-alanine gave 2-[(benzoylcarbamothioyl)amino]-3-hydroxypropanoic acid (I), 1-(benzoylcarbamothioyl)pyrrolidine-2-carboxylic acid (II), 2-[(benzoylcarbamothioyl)amino]-4-(methylsulfanyl)butanoic acid (III) and 2-[(benzoylcarbamothioyl)amino]propanoic acid (IV), respectively. The compounds have been characterized by IR, NMR, microanalyses and mass spectrometry. The crystal structures of all the compounds have also been discussed. Compound II showed rotamers in solution. DFT calculations of the frontier orbitals of the compounds have been carried out to ascertain the groups that contribute to the HOMO and LUMO, and to study their contribution to the reactivity of these compounds. The calculations indicated that the carboxylic acid group in these compounds is unreactive hence making the conversion to benzimidazoles via cyclization on the carboxylic acids impractical. This has been further confirmed by the reaction of compounds I-IV, respectively, with o-phenylene diamine which was unsuccessful but gave compound V.

  12. Synthesis and Bioactivity of N-Benzoyl-N'-[5-(2'-substituted phenyl-2-furoyl] Semicarbazide Derivatives

    Directory of Open Access Journals (Sweden)

    Zining Cui

    2010-06-01

    Full Text Available In order to find novel chitin synthesis inhibitors (CSIs with good activity, benzoylphenylurea, a typical kind of CSIs, was chosen as the lead compound and 15 novel derivatives containing furan moieties were designed by converting the urea linkage of benzoylphenylureas into a semicarbazide and changing the aniline part into furoyl groups. The title compounds were synthesized by the reaction of substituted benzoyl isocyanates with 5-(substituted phenyl-2-furoyl hydrazine, and the structures were confirmed by IR, 1H-NMR, elemental analysis and single crystal X-ray diffraction analyses (compound E2. The bioassay results indicated that the title compounds exhibit good insecticidal activity, especially towards Plutella xylostella L., but had lower fungicidal activity. Inspiringly, the title compounds possessed obvious anticancer activity against human promyelocytic leukemic cell line (HL-60, and some of the title compounds also had activity against human hepatocellular carcinoma cell line (Bel-7402, human gastric carcinoma cell line (BGC-823, and human nasopharyngeal carcinoma cell line (KB. The results indicated that the linkage in the lead compounds was important to the bioactivity and spectra. The modification on the urea linkage is an effective strategy to discover new pesticide and drug candidates.

  13. Design, synthesis and biological evaluation of 4-benzoyl-1-dichlorobenzoylthiosemicarbazides as potent Gram-positive antibacterial agents.

    Science.gov (United States)

    Paneth, Agata; Plech, Tomasz; Kaproń, Barbara; Hagel, Dominika; Kosikowska, Urszula; Kuśmierz, Edyta; Dzitko, Katarzyna; Paneth, Piotr

    2016-06-01

    Twelve 4-benzoyl-1-dichlorobenzoylthiosemicarbazides have been tested as potential antibacterials. All the compounds had MICs between 0.49 and 15.63 µg/ml toward Micrococcus luteus, Bacillus cereus, Bacillus subtilis and Staphylococcus epidermidis indicating, in most cases, equipotent or even more effective action than cefuroxime. In order to clarify if the observed antibacterial effects are universal, further research were undertaken to test inhibitory potency of two most potent compounds 3 and 11 on clinical isolates of Staphylococcus aureus. Compound 11 inhibited the growth of methicillin-sensitive S. aureus (MSSA) at MICs of 1.95-7.81 µg/ml, methicillin-resistant S. aureus (MRSA) at MICs of 0.49-1.95 µg/ml and MDR-MRSA at MIC of 0.98 and 3.90 µg/ml, respectively. Finally, inhibitory efficacy of 3 and 11 on planktonic cells and biofilms formation in clinical isolates of S. aureus and Haemophilus parainfluenzae was tested. The majority of cells in biofilm populations of MSSA and MRSA were eradicated at low level of 3, with MBICs in the range of 7.82-15.63 µg/ml. PMID:25897586

  14. Synthesis, spectroscopic characterization and photophysics of a novel environmentally sensitive dye 3-naphthyl-1-phenyl-5-(4-carboxyphenyl)-2-pyrazoline

    Energy Technology Data Exchange (ETDEWEB)

    Varghese, Beena; Al-Busafi, Saleh N.; Suliman, FakhrEldin O., E-mail: fsuliman@squ.edu.om; Al-Kindy, Salma M.Z., E-mail: alkindy@squ.edu.om

    2015-03-15

    Synthesis and photophysical properties of a novel pyrazoline – containing fluorophore, 3-naphthyl-1-phenyl-5-(4-carboxyphenyl)-2-pyrazoline (NPCP) A, and its proline derivative (NPCP-P) B are presented in this work. The highlight of this fluorescent dye is that, it can be prepared from available starting material via two synthetic steps, easily converted to the corresponding amide derivative by in situ nucleophilic acyl substitution of the corresponding acid chloride, and its purification by simple chromatographic techniques. The structures of the new compounds were verified using various spectroscopic tools. Furthermore, photophysical properties of the new fluorophores were studied and interesting solvatochromic behaviour was observed. Due to the presence of proton acceptor linked to the fluorophore, NPCP displays pH-sensitive absorption and fluorescence emission. The interaction of NPCP and NPCP-P with various micelles has been studied by steady state fluorescence. All results reflect the importance of the medium effect on the analytical application of NPCP as a potential fluorescent label for derivatization of analytes having amine (–NH{sub 2}) group. Theoretical calculations were performed for both compounds using time dependent density functional theory (TD-DFT) at B3LYP/6-31G(d, p) level. The calculations indicate that the exited state dipole moments are larger than those of the ground state in line with the experimental findings. - Highlights: • Synthesis of a naphthalene-pyrazoline fluorescence reagent for –NH{sub 2} containing compounds. • The fluorescence of the compounds exhibit interesting solvatochromism. • TD-DFT calculations at B3LYP/6-31G(d, p) was performed on the probe and its derivative.

  15. Synthesis, spectroscopic characterization and photophysics of a novel environmentally sensitive dye 3-naphthyl-1-phenyl-5-(4-carboxyphenyl)-2-pyrazoline

    International Nuclear Information System (INIS)

    Synthesis and photophysical properties of a novel pyrazoline – containing fluorophore, 3-naphthyl-1-phenyl-5-(4-carboxyphenyl)-2-pyrazoline (NPCP) A, and its proline derivative (NPCP-P) B are presented in this work. The highlight of this fluorescent dye is that, it can be prepared from available starting material via two synthetic steps, easily converted to the corresponding amide derivative by in situ nucleophilic acyl substitution of the corresponding acid chloride, and its purification by simple chromatographic techniques. The structures of the new compounds were verified using various spectroscopic tools. Furthermore, photophysical properties of the new fluorophores were studied and interesting solvatochromic behaviour was observed. Due to the presence of proton acceptor linked to the fluorophore, NPCP displays pH-sensitive absorption and fluorescence emission. The interaction of NPCP and NPCP-P with various micelles has been studied by steady state fluorescence. All results reflect the importance of the medium effect on the analytical application of NPCP as a potential fluorescent label for derivatization of analytes having amine (–NH2) group. Theoretical calculations were performed for both compounds using time dependent density functional theory (TD-DFT) at B3LYP/6-31G(d, p) level. The calculations indicate that the exited state dipole moments are larger than those of the ground state in line with the experimental findings. - Highlights: • Synthesis of a naphthalene-pyrazoline fluorescence reagent for –NH2 containing compounds. • The fluorescence of the compounds exhibit interesting solvatochromism. • TD-DFT calculations at B3LYP/6-31G(d, p) was performed on the probe and its derivative

  16. 1-(2-Methyl-5H-chromeno[2,3-b]pyridin-5-ylidene) hydrazone as fluorescent probes for selective zinc sensing in DMSO

    International Nuclear Information System (INIS)

    Two methyl-chromeno-pyridinylidene hydrazone derivatives L1, a cyclen derivative, and L2 were studied as potential fluorescent OFF–ON sensors towards Zn2+ in DMSO. Upon addition of one equivalent of Zn2+, L1 fluorescence was quenched, but addition of a second equivalent of Zn2+ restored partially the signal. Therefore ZnL1 behaved as a OFF–ON sensor for zinc. By comparison, L2 behaved as a very sensitive probe for zinc. ZnL1 and L2 sensor efficiencies were correlated to Zn2+ coordination via the hydrazone moiety of the fluorophore, which prevented a photoinduced electron transfer (PET), and allowed an efficient CHelation-Enhanced Fluorescence (CHEF) effect. -- Highlights: • According to Zn2+ concentration, L1 behaves as an on-off-on sensor. • Given that L1 concentration is known, its fluorescence response could give an immediate suggestion about the range of Zn2+ concentration. • L2 exhibited a strong fluorescence enhancement upon Zn2+ addition. • It was demonstrated that L2 was highly specific to Zn2+, which rendered this very straightforward ligand as an efficient and selective probe for this ion

  17. Polydopamine-based immobilization of a hydrazone covalent organic framework for headspace solid-phase microextraction of pyrethroids in vegetables and fruits.

    Science.gov (United States)

    Wu, Mingxue; Chen, Gang; Liu, Ping; Zhou, Weihong; Jia, Qiong

    2016-07-22

    We designed a novel hydrazone covalent organic framework (COF) and developed a polydopamine (PDA) method to immobilize COF on a stainless steel fiber for headspace solid-phase microextraction (HS-SPME). A series of characterization studies was performed to validate the structure and property of the prepared fiber. The COF-PDA fiber was applied for the extraction of pyrethroids coupled with gas chromatography equipped with an electron capture detector (GC-ECD). Under the optimum experimental conditions, high enhancement factors of 307-2327 were achieved, indicating that the hydrazone COF possessed good extraction efficiency for pyrethroids. The detection limits ranged from 0.11 to 0.23μgkg(-1) with relative standard deviations varying in the range of 3.6-9.2% (intra-batch) and 6.9-12.1% (inter-batch), respectively. The developed method was applied to the determination of pyrethroids in fruit and vegetable samples and the accuracy was assessed through recovery experiments. PMID:27317006

  18. 1-(2-Methyl-5H-chromeno[2,3-b]pyridin-5-ylidene) hydrazone as fluorescent probes for selective zinc sensing in DMSO

    Energy Technology Data Exchange (ETDEWEB)

    Nouri, Hela [URCA—Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, Groupe Chimie de Coordination, UFR Sciences, BP 1039, 51687 Reims Cedex 2 (France); LACReSNE—Université de Carthage, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte (Tunisia); Cadiou, Cyril, E-mail: cyril.cadiou@univ-reims.fr [URCA—Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, Groupe Chimie de Coordination, UFR Sciences, BP 1039, 51687 Reims Cedex 2 (France); Henry, Axelle; Déchamps-Olivier, Isabelle [URCA—Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, Groupe Chimie de Coordination, UFR Sciences, BP 1039, 51687 Reims Cedex 2 (France); Ternane, Riadh; Trabelsi-Ayadi, Malika [LACReSNE—Université de Carthage, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte (Tunisia); Lemercier, Gilles; Chuburu, Françoise [URCA—Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, Groupe Chimie de Coordination, UFR Sciences, BP 1039, 51687 Reims Cedex 2 (France)

    2014-04-15

    Two methyl-chromeno-pyridinylidene hydrazone derivatives L1, a cyclen derivative, and L2 were studied as potential fluorescent OFF–ON sensors towards Zn{sup 2+} in DMSO. Upon addition of one equivalent of Zn{sup 2+}, L1 fluorescence was quenched, but addition of a second equivalent of Zn{sup 2+} restored partially the signal. Therefore ZnL1 behaved as a OFF–ON sensor for zinc. By comparison, L2 behaved as a very sensitive probe for zinc. ZnL1 and L2 sensor efficiencies were correlated to Zn{sup 2+} coordination via the hydrazone moiety of the fluorophore, which prevented a photoinduced electron transfer (PET), and allowed an efficient CHelation-Enhanced Fluorescence (CHEF) effect. -- Highlights: • According to Zn{sup 2+} concentration, L1 behaves as an on-off-on sensor. • Given that L1 concentration is known, its fluorescence response could give an immediate suggestion about the range of Zn{sup 2+} concentration. • L2 exhibited a strong fluorescence enhancement upon Zn{sup 2+} addition. • It was demonstrated that L2 was highly specific to Zn{sup 2+}, which rendered this very straightforward ligand as an efficient and selective probe for this ion.

  19. Spectrophotometric Determination of Cu2+ and Monitoring of Hg2+ and Ni2+ in some Iranian Vegetables Using 6-(2-Naphthyl)-2, 3-Dihydro-as-triazine-3-thione

    OpenAIRE

    Shamsa, Fazel; Barazande Tehrani, Malehe; Mehravar, Hamid; MOHAMMADI, ELAHEH

    2013-01-01

    Recently, 6-(2-naphthyl)-2, 3-dihydro-as-triazine-3-thione (NDTT) was synthesized in laboratory and used successfully for the spectrophotometric determination of nanogram levels of Cu2+ in aqueous solution. This reagent forms a specific red complex with Cu2+ ions after the extraction by chloroform at alkaline pH. The absorption of the complex in the UV region (313 nm) is about 8 times as strong as in the visible one (510 nm). Mercury and nickel ions form yellow complexes with NDTT under the s...

  20. Antischistosomal activity of acridanone- hydrazones in Cebus monkeys experimentally infected with the SJ strain of Schistosoma mansoni

    Directory of Open Access Journals (Sweden)

    Paulo Marcos Zech Coelho

    1995-09-01

    Full Text Available In this study, four compounds were utilized at the dose of 12.5mg/kg body weight, p.o., to treat Cebus monkeys experimentally infected with about 200 cercariae of Schistosoma mansoni (SJ strain, via transcutaneous route. The oograms performed with rectal snips, as well as stool examinations carried out periodically, showed no viable eggs of the parasite, from day 29 to 226post-treatment. The perfusion undertaken after killing the animals showed absence of worms in the treated monkeys, whereas 83 worms were recovered from the control, thus corroborating the results obtained by means of oograms and coproscopy. These results confirm the efficacy of 9-acridanone- hydrazones previously tested against the LE strain of S. mansoni. The low curative dose and apparent absence of toxicity render these dmgs an important therapeutic reserve, taking into consideration the reports on the resistance of S. mansoni to the modern drugs oxamniquine and praziquantel.No presente trabalho, quatro compostos foram utilizados na dose de 12,5mg/kg de peso, por via oral, em macacos infectados transcutaneamente com cerca de 200 cercárias de Schistosoma mansoni. Os oogramas realizados com fragmentos de mucosa retal e os exames de fezes realizados, periodicamente, demonstraram a ausência de ovos viáveis do parasito a partir do 29- até o 226a dia pós-tratamento. A perfusão, apôs sacrifício dos animais tratados, não detectou vermes, enquanto que do macaco cotztrole 83 vermes foram recuperados, confirmando assim os resultados dos oogramas e da coproscopia. Estes resultados confirmam a eficácia das 9-acridanonas- hydrazonas já observada anteriormente contra a cepa LE de S. mansoni. A baixa dosagem curativa e aparente ausência de toxicidade colocam estas drogas como uma reserva terapêutica importante, tendo em vista o relato de resistência do S. mansoni às drogas modernas oxamniquína e praziquantel.

  1. Extraction-spectrophotometric determination of vanadium in stainless steel and nickel-base alloys with N-benzoyl-N-phenylhydroxylamine

    International Nuclear Information System (INIS)

    A simple, rapid, and accurate extraction-spectrophotometric methods has been developed for the determination of vanadium in stainless steel and Ni-base alloys. The procedure is as follows: Take 0.5 g of sample into a beaker and add 20 ml of aqua regia, then heat and dissolve it. Furthermore add 5 ml of perchloric acid, and heat until the sample is dissolved, and add 14 ml of sulfuric acid (1 + 1) and 5 ml of phosphoric acid. Continue heating untill fumes of sulfuric acid generate from it. Thereafter, transfer it with use of water into a polyethylene separating funnel, add 10 ml of hydrofluoric acid (46%) and dilute to 50 ml with water. Then, add 4 ml of iron (II) ammonium sulfate solution (10%) and mix it thoroughly. Allow to stand for two or three min, and add 10 ml of ammonium peroxy-sulfate solution (45%) and mix it thoroughly again. By this procedure vanadium is oxidized to vanadium (V) without any oxidation of chromium (III). Allow to stand for about five minutes. Then add exactly 20 ml of N-benzoyl-N-phenylhydroxylamine chloroform solution (0.1%) and shake it vigorously for two min. Then, determine vanadium by measuring absorbance at the wavelength of 530 nm against a chloroform reference. The interference of chromium can be eliminated by reduction to Cr (III) with iron (II) ammonium sulfate, while manganese and molybdenum do not interfere at 530 nm. In the determination of 100 μg vanadium, the following amounts of foreign ions are tolerated: Fe (III) and Ni 1 g, Cr (III) 500 mg, Al 200 mg, Mo (VI) 100 mg, Mn, Co (II), Ti (IV) and Nb (V) 50 mg, Si 20 mg, Cu 10 mg, Ta (V) and W (VI) 5 mg. (author)

  2. Synthesis of n, n-bis(benzoyl) azelaic acid dihydrazide and its effect on performance of poly (l-lactic acid)

    International Nuclear Information System (INIS)

    In order to synthesize more function amides, N, N-bis(benzoyl) azelaic acid dihydrazide(NA(A)) was synthesized from benzoyl hydrazine and azelaoyl chloride which was deprived from azelaic acid via acylation. The influence of the reaction ratio, reaction time and reaction temperature to the yield of NA(A) was investigated by orthogonal experiment, the optimization result was: molar ratio of benzoyl hydrazine: azelaoyl chloride 2:3, reaction time 6 h, reaction temperature 70 degree C.The yield was 89.7%. Non-isothermal crystallization behavior measure indicated that NA(A) showed excellent nucleating effects on Poly(L-lactic acid)(PLLA) crystallization. Compared to the neat PLLA, with the addition of 0.8% NA(A), the crystallization temperature increased from 105.88 degree to 122.99 degree C,the degree of supercooling decreased from 55.33 degree C to 36.96 degree C while the crystallization enthalpy increased from 1.379 Jog/sup -1/ to 28.58 Jog/sup -1/ at a cooling rate of 1degree C/min from melt. The tensile strengths and tensile modulus increased with the increasing of NA(A) contents and possessed a maximum value for the critical NA(A) loading 0.3% and 0.5%, respectively. However, the elongations at break of PLLA/NA(A) samples decreased significantly. The hardness of PLLA/NA(A) samples after isothermal crystallization increased, and the largest value of hardness of PLLA/NA(A) with 1%NA(A) after isothermal crystallization was 176N/mm/sup 2/. (author)

  3. Dimethyl-Aluminium Complexes Bearing Naphthyl-Substituted Pyridine-Alkylamides as Pro-Initiators for the Efficient ROP of ε-Caprolactone

    Directory of Open Access Journals (Sweden)

    Andrew P. Armitage

    2015-08-01

    Full Text Available Three sterically-enhanced 2-imino-6-(1-naphthylpyridines, 2-{CMe=N(Ar}-6-(1-C10H7C5H3N [Ar = 2,6-i-Pr2C6H3 (L1dipp, 2,4,6-i-Pr3C6H2 (L1tripp, 4-Br-2,6-i-Pr2C6H2 (L1Brdipp], differing only in the electronic properties of the N-aryl group, have been prepared in high yield by the condensation reaction of 2-{CMe=O}-6-(1-C10H7C5H3N with the corresponding aniline. Treatment of L1dipp, L1tripp and L1Brdipp with two equivalents of AlMe3 at elevated temperature affords the distorted tetrahedral 2-(amido-prop-2-yl-6-(1-naphthylpyridine aluminum dimethyl complexes, [2-{CMe2N(Ar}-6-(1-C10H7C5H3N]AlMe2 [Ar = 2,6-i-Pr2C6H3 (1a, 2,4,6-i-Pr3C6H2 (1b, 4-Br-2,6-i-Pr2C6H2 (1c], in good yield. The X-ray structures of 1a–1c reveal that complexation has resulted in concomitant C–C bond formation via methyl migration from aluminum to the corresponding imino carbon in L1aryl; in solution, the restricted rotation of the pendant naphthyl group in 1 confers inequivalent methyl ligand environments. The ring opening polymerization of ε-caprolactone employing 1, in the presence of benzyl alcohol, proceeded efficiently at 30 °C producing polymers of narrow molecular weight distribution with the catalytic activities dependent on the nature of the substituent located at the 4-position of the N-aryl group with the most electron donating i-Pr derivative exhibiting the highest activity (1b > 1a > 1c; at 50 °C 1b mediates 100% conversion of the monomer to polycaprolactone (poly(CL in one hour. In addition to 1a, 1b and 1c, the single crystal X-ray structures are reported for L1dipp and L1tripp.

  4. THE STRUCTURE OF 3,5-DI-O-BENZOYL-1,2-DIDEOXY-1-PHENYL-BETA-D-RIBOFURANOSE, C25H22O5

    OpenAIRE

    GUNNING, J.; Neidle, S; MILLICAN, T.; Eaton, M; MOCK, G.; Mann, J.

    1985-01-01

    Mr=402.4, orthorhombic, P212~2 l, a= 4-946 (1), b= 15.887 (2), c=26.555 (2)A, V= 2086.7 (5) A 3, Z = 4, D x = 1.28 gcm -a, Cu Ka, 2 = 1.5418/k, B = 6.868 cm -1, F(000) = 848, T= 293 K, final R =0.054 for 648 observed reflections. The molecule is propeller shaped. The benzoyl groups act as protecting groups and the phenyl group is a base substitute. The crystal structure does not involve any intermolecular stacking interactions between the phenyl groups. The molecule...

  5. Synthesis of a Novel Benzoyl Adenosine Analog Containing a 1, 4-Dioxane Sugar Analog and the Synthesis of a Corresponding Uracil Adenine Dinucleotide

    Directory of Open Access Journals (Sweden)

    Per Carlsen

    2011-05-01

    Full Text Available Adenosine analogs in which the sugar unit was replaced by a 1,4-dioxane sugar equivalent, were prepared by coupling the 1,4-dioxane sugar analog as its anomeric acetates, with N6-benzoyl protected adenine. The 1,4-dioxane system was obtained in an enantioselective synthesis from (R,R-dimethyl tartrate. Using standard phosphorimidite methodology, the adenine analog was further reacted with a 1,4-dioxane uridine analog to give the corresponding, protected dinucleotide, set-up for further condensation into larger oligonucleotides.

  6. N-(4-Substituted-benzoyl)-N'-(beta-d-glucopyranosyl)ureas as inhibitors of glycogen phosphorylase: Synthesis and evaluation by kinetic, crystallographic, and molecular modelling methods

    OpenAIRE

    Veronika Nagy; Nora Felfoeldi; Balint Konya; Praly, Jean-Pierre; Tibor Docsa; Pal Gergely; Chrysina, Evangelia D.; Tiraidis, Costas; Kosmopoulou, Magda N.; Alexacou, Kyra-Melinda; Konstantakaki, Maria; Leonidas, Demetres D.; Zographos, Spyros E.; Oikonomakos, Nikos G.; Kozmon, Stanislav

    2012-01-01

    N-(4-Substituted-benzoyl)-N'-(beta-D-glucopyranosyl)ureas (substituents: Me, Ph, Cl, OH, OMe, NO2, NH2, COOH, and COOMe) were synthesised by ZnCl2 catalysed acylation of O-peracetylated beta-D-glucopyranosyl urea as well as in reactions of O-peracetylated or O-unprotected glucopyranosylamines and acyl-isocyanates. O-deprotections were carried out by base or acid catalysed transesterifications where necessary. Kinetic studies revealed that most of these compounds were low micromolar inhibitors...

  7. Potentiometric studies on the chelation behaviour of ω-benzoyl-2-hydroxy-4-methoxy-3-methyl-acetophenone (BHMMA) with lanthanons

    International Nuclear Information System (INIS)

    The chelation behaviour of complexes of La(3), Pr(3), Nd(3), Sm(3), Y(3), Tb(3), Dy(3), Ho(3) with ω-benzoyl-2-hydroxy-4-methoxy-3-methyl-acetophenone has been studied potentiometrically in 75% (v/v) aqueous alcohol medium at various ionic strengths. The method of Bjerrum and Calvin, as modified by Irving and Rossotti, has been used to find values of n-bar and pL. The stability constants and the values of Smin have been calculated. The order of stability constants was found to be: La < Pr < Nd < Sm < Y < Tb < Dy < Ho. (Author)

  8. 光度法测定小麦粉中过氧化苯甲酰研究%Spectrophotometric Determination of Flour Benzoyl Peroxide

    Institute of Scientific and Technical Information of China (English)

    田林双; 于伟; 吴存兵; 顾鹏程; 周琳琨; 邱琳

    2013-01-01

    基于过氧化苯甲酰的氧化性,将Fe2+氧化成Fe3+,生成的Fe3+与硫氰酸盐在酸性乙醇介质中发生显色反应,建立小麦粉违禁添加剂过氧化苯甲酰检测新方法.对该方法进行试验条件研究,包括光谱吸收曲线、反应介质、酸含量、反应温度、反应时间、Fe2浓度、KSCN浓度、共存干扰物质等因素对检测结果的影响.最佳试验条件下,过氧化苯甲酰线性范围0.1~15 mg/L,相关系数R2=0.999 4,505 nm处表观摩尔吸光系数ε =2.136 5×104 L·mol-1·cm-1,检出限0.025 mg/L.利用该方法对市售小麦粉样品进行测定,回收率在97.2%~104.4%之间.%A new method for benzoyl peroxide detection was proposed.It was based on the principle that benzoyl peroxide oxidize ferrous iron to ferric ion,then color reaction between ferric ion and thiocyanate in ethanol and acid system can be quantified.Experimental conditions of the benzoyl peroxide detection method including absorption curve,reaction medium,acid content,reaction temperature,reaction time,ferrous iron content,thiocyanate content and interfering substances were studied in the research.Under the optimum conditions,the linear range of benzoyl peroxide concentration was 0.1 ~ 15 mg/L,with a correlation coefficient (R2) of 0.999 4 and a lower detection limit of 0.025 mg/L.The apparent molar adsorptivity of the coordination complex was 2.136 5 × 104 L · mol-1 · cm-1The recovery was at the range of 97.2% to 104.4% by this method to detect commercial flour samples.

  9. Sub-group Analyses from a Trial of a Fixed Combination of Clindamycin Phosphate 1.2% and Benzoyl Peroxide 3.75% Gel for the Treatment of Moderate-to-severe Acne Vulgaris

    Science.gov (United States)

    Korotzer, Andrew

    2015-01-01

    Background: Acne vulgaris is commonplace and can be difficult to manage. Providing an effective and well-tolerated treatment may lead to improved adherence, increased patient satisfaction, and improved clinical outcomes. Methods: A review of efficacy, safety, and cutaneous tolerability of clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel in 498 patients with moderate-to-severe acne vulgaris enrolled in a multicenter Phase III study randomized to receive active or vehicle once daily for 12 weeks, including the most recent post-hoc analyses. Results: Significantly superior reductions in lesion counts were observed with clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel from Week 4, with median percent reductions in inflammatory and noninflammatory lesions from baseline of 68.4 and 57.9 percent, respectively (bothp<0.001 versus vehicle). More than half (55.1%) of the severe acne vulgaris patients treated with clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel achieved ≥2-grade improvement from baseline in their Evaluator’s Global Severity Score, and almost a third of the adolescent acne vulgaris patients (32.4%) achieved at least a marked improvement in their acne vulgaris as early as Week 2. In adult female acne overall treatments success was achieved in 52.7 percent of patients treated with clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel. Overall, and in the specific subpopulations, clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel was well-tolerated with a similar adverse event profile to vehicle. Limitations: Post-hoc analyses from a single clinical trial with demographic imbalances that could potentially confound the results. Conclusion: Clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel appears to be effective in treating acne across various clinically relevant sub-groups. PMID:26705445

  10. NMR and DFT Calculation Study on Structures of 2-[2-nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC) and Its Two Metabolites Isolated from Urine of Patients Suffering from Tyrosinemia Type I.

    OpenAIRE

    Gryff-Keller, Adam; Szczeciński, Przemysław; Kraska-Dziadecka, Anna

    2010-01-01

    Abstract 2-[2-Nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC) is an active component of nitisinone, a medicine against tyrosinemia type I. Using 1H, 13C and 19F NMR spectroscopy it has been found that in urine of patients treated with nitisinone two compounds possessing CF3 group are always present. They have been isolated by TLC technique and identified as 4-hydroxy-2-[2-nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione and 5-hydroxy-2-[2-nitro-4-(trifluoromethy...

  11. Identification of 2-[2-nitro-4-(trifluoromethyl)benzoyl]- cyclohexane-1,3-dione metabolites in urine of patients suffering from tyrosinemia type I with the use of 1H and 19F NMR spectroscopy.

    Science.gov (United States)

    Szczeciński, Przemysław; Lamparska, Diana; Gryff-Keller, Adam; Gradowska, Wanda

    2008-01-01

    Organic extracts of six urine samples from children treated with nitisinone, a medicine against tyrosinemia type I, were investigated by (1)H and (19)F NMR spectroscopy. The presence of unchanged 2-[2-nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC), 6-hydroxy-2-[2-nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC-OH) and 2-nitro-4-trifluoromethylbenzoic acid (NTFA) as well as a few other unidentified compounds containing CF(3) group was documented. PMID:19039335

  12. Identification of 2-[2-nitro-4-(trifluoromethyl)benzoyl]-cyclohexane-1,3-dione metabolites in urine of patients suffering from tyrosinemia type I with the use of 1H and 19F NMR spectroscopy

    International Nuclear Information System (INIS)

    Organic extracts of six urine samples from children treated with nitisinone, a medicine against tyrosinemia type I, were investigated by 1H and 19F NMR spectroscopy. The presence of unchanged 2-[2-nitro-4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC), 6-hydroxy-2-[2-nitro- 4-(trifluoromethyl)benzoyl]cyclohexane-1,3-dione (NTBC-OH) and 2-nitro-4-trifluoromethylbenzoic acid (NTFA) as well as a few other unidentified compounds containing CF3 group was documented. (authors)

  13. Facile green synthesis and potent antimicrobial efficacy of -aminoheteronapthol via tailored Betti’s protocol and their bis-aryl hydrazone click products

    Indian Academy of Sciences (India)

    K M Khandarkar; M D Shanti; M Ahmed; J S Meshram

    2013-11-01

    A series of novel Mannich base and their hydrazone derivatives were synthesized by highly resourceful, chic, simple and green technique with exceptionally facile reaction conditions of one-pot, three component reaction with an array of biologically and pharmaceutically active novel heterocycles. The protocol offers a valuable alternative to known methods and will find applications in the field of green synthesis and antimicrobial study against pathogenic microbes, supporting the development of bioinformatical database of novel and derelict heterocycles. These data indicate their potential to become antifungal agents. The novel products were established by elemental, IR, mass spectroscopic and NMR analysis. The environmental advantages of the method include short reaction time, excellent yield, easy work-up, absence of extraction and chromatographic purification steps.

  14. MICROWAVE ASSISTED SYNTHESIS OF 3-(2-BENZOYL-6-HYDROXY-3-METHYL BENZO[b] FURAN-5-YL-5-(ARYL-4, 5-DIHYDRO-1H-PYRAZOLE CARBOTHIOAMIDES AND THEIR ANTIBACTERIAL ACTIVITY Mikrowellen unterstützte Synthese von 3 - (2-Benzoyl-6-HYDROXY-3-METHYL Benzo [b] furan-5-yl -5 - (ARYL -4, 5-DIHYDRO-1H-pyrazol CARBOTHIOAMIDES UND ihre antibakterielle Aktivität

    Directory of Open Access Journals (Sweden)

    Ashok D, Sudershan K,Khalilullah M

    2011-10-01

    Full Text Available A series of 3-(2-Benzoyl-6-hydroxy-3-methyl benzo[b] furan-5-yl-5-(aryl-4, 5-dihydro-1Hpyrazole carbothioamides have been prepared by the reaction of (E-1-(2-Benzoyl-6-hydroxy-3- methylbenzo[b]furan-5-yl-3-aryl-2-propen-1-ones with thiosemicarbazide in the presence of sodium hydroxide under microwave irradiation. The structures of newly synthesized compounds have been confirmed on the basis of elemental analysis, IR,1H-NMR,13C-NMR and mass spectral data. All the compounds were screened for their antibacterial activity.

  15. An Eco-Friendly Ultrasound-Assisted Synthesis of Novel Fluorinated Pyridinium Salts-Based Hydrazones and Antimicrobial and Antitumor Screening

    Directory of Open Access Journals (Sweden)

    Nadjet Rezki

    2016-05-01

    Full Text Available The present work reports an efficient synthesis of fluorinated pyridinium salts-based hydrazones under both conventional and eco-friendly ultrasound procedures. The synthetic approach first involves the preparation of halogenated pyridinium salts through the condensation of isonicotinic acid hydrazide (1 with p-fluorobenzaldehyde (2 followed by the nucleophilic alkylation of the resulting N-(4-fluorobenzylideneisonicotinohydrazide (3 with a different alkyl iodide. The iodide counteranion of 5–10 was subjected to an anion exchange metathesis reaction in the presence of an excess of the appropriate metal salts to afford a new series of fluorinated pyridinium salts tethering a hydrazone linkage 11–40. Ultrasound irradiation led to higher yields in considerably less time than the conventional methods. The newly synthesized ILs were well-characterized with FT-IR, 1H NMR, 13C NMR, 11B, 19F, 31P and mass spectral analyses. The ILs were also screened for their antimicrobial and antitumor activities. Within the series, the salts tethering fluorinated counter anions 11–13, 21–23, 31–33 and 36–38 were found to be more potent against all bacterial and fungal strains at MIC 4–8 µg/mL. The in vitro antiproliferative activity was also investigated against four tumor cell lines (human ductal breast epithelial tumor T47D, human breast adenocarcinoma MCF-7, human epithelial carcinoma HeLa and human epithelial colorectal adenocarcinoma Caco-2 using the MTT assay, which revealed that promising antitumor activity was exhibited by compounds 5, 12 and 14.

  16. Synthesis, biological evaluation, drug-likeness, and in silico screening of novel benzylidene-hydrazone analogues as small molecule anticancer agents.

    Science.gov (United States)

    Alam, Mohammad Sayed; Lee, Dong-Ung

    2016-02-01

    A series of fifteen benzylidene-hydrazone analogues (3a-o), including eight new compounds, were synthesized and evaluated for their cytotoxic activities in four human cancer cell lines and for their antioxidant activities using DPPH. Of the tested compounds 3e, which possesses two methoxy substituents in its benzylidene phenyl ring, was found to be potently cytotoxic to all cancer cell lines tested with IC50 values of 0.12 (lung), 0.024 (ovarian), 0.097 (melanoma), and 0.05 μM (colon), and these IC50 values were comparable to those of the doxorubicin standard (IC50 = 0.021, 0.074, 0.001, and 0.872 μM, respectively). DPPH assay showed compounds 3f, 3i, and 3g had IC50 values of 0.60, 0.99, and 1.30 μM, respectively, which were comparable to that of ascorbic acid (IC50 = 0.87 μM). Computational parameters such as, drug-likeness, ADME properties, toxicity effects, and drug scores were evaluated, and none of the fifteen compounds violated Lipinski's rule of five or Veber's rule, and thus they demonstrated good drug-likeness properties. In addition, all fifteen compounds had a higher drug score than the doxorubicin and BIBR1532. In silico screening was also conducted by docking of the active compounds on the active site of telomerase reverse transcriptase catalytic subunit, an important therapeutic target of anticancer agents, to determine the probable binding properties. The total binding energies of docked compounds are correlated well with cytotoxic potencies (pIC50) against lung, ovarian, melanoma, and colon cancer cell lines indicating that the benzylidene-hydrazones could use for the development of new anticancer agents as a telomerase inhibitor. PMID:26694484

  17. The isolated perfused bovine udder as an in vitro model of percutaneous drug absorption. Skin viability and percutaneous absorption of dexamethasone, benzoyl peroxide, and etofenamate.

    Science.gov (United States)

    Kietzmann, M; Löscher, W; Arens, D; Maass, P; Lubach, D

    1993-10-01

    Using udders from slaughtered cows as a new in vitro model of percutaneous drug absorption, the tissue viability and the percutaneous absorption of dexamethasone, benzoyl peroxide, and etofenamate were studied. The organ was perfused with gassed tyrode solution for up to 6 hr. As shown by measurement of glucose consumption, lactate production, lactate dehydrogenase activity, and pH in the perfusate, the tissue was viable over a 6-hr period. This was confirmed by a histological examination. Determination of the udder skin-fold thickness demonstrated that no edema developed within the perfusion period. A maximum skin penetration of dexamethasone was found after administration of dexamethasone dissolved in acetone with dimethyl sulfoxide, followed by ointment with salicylic acid, ointment without salicylic acid, and acetone solution. Experiments with benzoyl peroxide and etofenamate demonstrated that the perfused udder skin was capable of metabolizing drugs in vitro. In conclusion, the isolated perfused bovine udder is a new in vitro model, which maintains bovine udder skin with an isolated vasculature in a viable state. Using this in vitro model, we note it is possible to compare the dermal penetration, metabolism, and absorption of substances after topical administration of different drug formulations. PMID:8298184

  18. N-(4-Substituted-benzoyl)-N'-(β-d-glucopyranosyl)ureas as inhibitors of glycogen phosphorylase: Synthesis and evaluation by kinetic, crystallographic, and molecular modelling methods.

    Science.gov (United States)

    Nagy, Veronika; Felföldi, Nóra; Kónya, Bálint; Praly, Jean-Pierre; Docsa, Tibor; Gergely, Pál; Chrysina, Evangelia D; Tiraidis, Costas; Kosmopoulou, Magda N; Alexacou, Kyra-Melinda; Konstantakaki, Maria; Leonidas, Demetres D; Zographos, Spyros E; Oikonomakos, Nikos G; Kozmon, Stanislav; Tvaroška, Igor; Somsák, László

    2012-03-01

    N-(4-Substituted-benzoyl)-N'-(β-d-glucopyranosyl) ureas (substituents: Me, Ph, Cl, OH, OMe, NO(2), NH(2), COOH, and COOMe) were synthesised by ZnCl(2) catalysed acylation of O-peracetylated β-d-glucopyranosyl urea as well as in reactions of O-peracetylated or O-unprotected glucopyranosylamines and acyl-isocyanates. O-deprotections were carried out by base or acid catalysed transesterifications where necessary. Kinetic studies revealed that most of these compounds were low micromolar inhibitors of rabbit muscle glycogen phosphorylase b (RMGPb). The best inhibitor was the 4-methylbenzoyl compound (K(i)=2.3μM). Crystallographic analyses of complexes of several of the compounds with RMGPb showed that the analogues exploited, together with water molecules, the available space at the β-pocket subsite and induced a more extended shift of the 280s loop compared to RMGPb in complex with the unsubstituted benzoyl urea. The results suggest the key role of the water molecules in ligand binding and structure-based ligand design. Molecular docking study of selected inhibitors was done to show the ability of the binding affinity prediction. The binding affinity of the highest scored docked poses was calculated and correlated with experimentally measured K(i) values. Results show that correlation is high with the R-squared (R(2)) coefficient over 0.9. PMID:22325154

  19. Stabilization of the bicontinuous cubic phase in siloxane-terminated mesogens, 1,2-bis[4'-(n-(oligodimethylsiloxyl)alkoxy)benzoyl]hydrazine.

    Science.gov (United States)

    Kutsumizu, Shoichi; Tokiwa, Issei; Kawafuchi, Akane; Miwa, Yohei; Yamamura, Yasuhisa; Saito, Kazuya

    2016-03-23

    The introduction of oligodimethyl siloxane segments at the termini of the alkyl tails has been employed to stabilize the bicontinuous cubic (Cubbi) phase of a chain-core-chain type molecule having a 1,2-bis(benzoyl)hydrazine central core with two chains attached at the 4' position of each benzoyl moiety. In this study, three silylated molecules, , , and , were synthesized, where "CnSim" represents the number of carbon and silicon atoms in the chain and "bis" indicates the two chains being the same, whereas the last one is asymmetric with respect to the core. The phase behaviors were examined by using polarized optical microscopy, differential scanning calorimetry, and X-ray diffraction techniques. All three compounds form Cubbi phases and their syntheses were compared including their parent compound . It was clearly revealed that the introduction of oligodimethyl siloxane segments effectively suppresses the crystallization at low temperatures, and as a result stabilizes the Cubbi phases, in an extreme case down to room temperature. The semi-quantitative analyses in terms of lattice constant and three-dimensional electron density map help us to better understand the self-assembly process in the Cubbi phases. The study also revealed that the introduction of oligodimethyl siloxane segments is not only an alternative for the hydrocarbon segment but also is able to provide a versatile design strategy for obtaining stable Cubbi phases. PMID:26965052

  20. Formulation and evaluation of a topical niosomal gel containing a combination of benzoyl peroxide and tretinoin for antiacne activity

    Directory of Open Access Journals (Sweden)

    Gupta A

    2014-12-01

    Full Text Available Ankush Gupta,1,* Sima Singh,1,* Niranjan G Kotla,1 Thomas J Webster2,3 1Department of Pharmaceutical Sciences, Lovely Professional University, Phagwara, Punjab, India; 2Department of Chemical Engineering, Northeastern University, Boston, MA, USA; 3Center of Excellence for Advanced Materials Research, King Abdulaziz University, Jeddah, Saudi Arabia *These authors contributed equally to this work Abstract: A skin disease, like acne, is very common and normally happens to everyone at least once in their lifetime. The structure of the stratum corneum is often compared with a brick wall, with corneocytes surrounded by the mortar of the intercellular lipid lamellae. One of the best options for successful drug delivery to the affected area of skin is the use of elastic vesicles (niosomes which can be transported through the skin through channel-like structures. In this study, a combination of tretinoin (keratolytic agent and benzoyl peroxide (BPO (a potent antibacterial was given by using niosomes as promising carriers for the effective treatment of acne by acting on a pathogenic site. In this section, niosomal gel formulation encapsulated drugs have been evaluated for in vitro, ex vivo, and in vivo, for their predetermined characteristics; and finally the stability of the niosome gel was tested at different temperature conditions for understanding of the storage conditions required for maintaining the quality of formulation attributes. The prepared niosome was found to be in the range of 531 nm with a zeta potential of -43 mV; the entrapment efficiencies of tretinoin (TRA and BPO niosomes were found to be 96.25%±0.56% and 98.75%±1.25%, respectively. The permeated amount of TRA and BPO from the niosomal gel after 24 hours was calculated as 6.25±0.14 µg/cm2 and 5.04±0.014 µg/cm2, respectively. A comparative drug retention study in Wistar rat skin using cream, an alcoholic solution, and a niosomal gel showed 11.54 µg, 2.68 µg, and 15.54 µg

  1. Determination of the Tautomeric Equilibria of Pyridoyl Benzoyl -Diketones in the Liquid and Solid State through the use of Deuterium Isotope Effects on 1H and 13C NMR Chemical Shifts and Spin Coupling Constants

    DEFF Research Database (Denmark)

    Hansen, Poul Erik; Borisov, Eugeny V.; Lindon, John C.

    2015-01-01

    The tautomeric equilibria for 2-pyridoyl-, 3-pyridoyl-, and 4-pyridoyl-benzoyl methane have been investigated using deuterium isotope effects on 1H and 13C chemical shifts both in the liquid and the solid state. Equilibria are established both in the liquid and the solid state. In addition, in th...

  2. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases; Cromatografia en fase gaseosa sobre metilfenilpolisiloxanos. Estructura molecular y parametros de retencion para alcoholes y sus derivados benzoilados

    Energy Technology Data Exchange (ETDEWEB)

    Pias, J. B.; Gasco, L.

    1976-07-01

    The retention indices of aliphatic alcohols of carbon number up to C{sub g}, and of their benzoyl derivatives up to C{sub 7}, were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH{sub 2}- group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices {delta}l , and positional and structural increments {delta}I, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs.

  3. Kinetics of hydrolysis of 1-benzoyl-1,2,4-triazole in aqueous solution as a function of temperature near the temperature of maximum density, and the isochoric controversy

    NARCIS (Netherlands)

    Blandamer, MJ; Buurma, NJ; Engberts, JBFN; Reis, JCR; Buurma, Niklaas J.; Reis, João C.R.

    2003-01-01

    At temperatures above and below the temperature of maximum density, TMD, for water at ambient pressure, pairs of temperatures exist at which the molar volumes of water are equal. First-order rate constants for the pH-independent hydrolysis of 1-benzoyl-1,2,4-triazole in aqueous solution at pairs of

  4. Benzoyl Peroxide Topical

    Science.gov (United States)

    ... cosmetics or soaps that dry the skin, medicated cosmetics, sunlight, and sunlamps) unless directed otherwise by your doctor.It may take 4 to 6 weeks to see the effects of this medication. If your acne does not ...

  5. Spectrophotometric Determination of Cu2+ and Monitoring of Hg2+ and Ni2+ in some Iranian Vegetables Using 6-(2-Naphthyl)-2, 3-Dihydro-as-triazine-3-thione

    Science.gov (United States)

    Shamsa, Fazel; Barazande Tehrani, Malehe; Mehravar, Hamid; Mohammadi, Elaheh

    2013-01-01

    Recently, 6-(2-naphthyl)-2, 3-dihydro-as-triazine-3-thione (NDTT) was synthesized in laboratory and used successfully for the spectrophotometric determination of nanogram levels of Cu2+ in aqueous solution. This reagent forms a specific red complex with Cu2+ ions after the extraction by chloroform at alkaline pH. The absorption of the complex in the UV region (313 nm) is about 8 times as strong as in the visible one (510 nm). Mercury and nickel ions form yellow complexes with NDTT under the same conditions which interfere in the UV region and without effect on Cu (II) absorbance in the visible region. The studied vegetables include Mentha pipereta L., Anethum graveolens L., Beta vulgaris L., Coriandrum sativum, Petroselinum hortense H., Ocimum basilicum L., Spinacia oleracea L., Lactuca sativa L., and Brassica oleracea L. PMID:24250566

  6. Spectrophotometric Determination of Cu(2+) and Monitoring of Hg(2+) and Ni(2+) in some Iranian Vegetables Using 6-(2-Naphthyl)-2, 3-Dihydro-as-triazine-3-thione.

    Science.gov (United States)

    Shamsa, Fazel; Barazande Tehrani, Malehe; Mehravar, Hamid; Mohammadi, Elaheh

    2013-01-01

    Recently, 6-(2-naphthyl)-2, 3-dihydro-as-triazine-3-thione (NDTT) was synthesized in laboratory and used successfully for the spectrophotometric determination of nanogram levels of Cu(2+) in aqueous solution. This reagent forms a specific red complex with Cu(2+) ions after the extraction by chloroform at alkaline pH. The absorption of the complex in the UV region (313 nm) is about 8 times as strong as in the visible one (510 nm). Mercury and nickel ions form yellow complexes with NDTT under the same conditions which interfere in the UV region and without effect on Cu (II) absorbance in the visible region. The studied vegetables include Mentha pipereta L., Anethum graveolens L., Beta vulgaris L., Coriandrum sativum, Petroselinum hortense H., Ocimum basilicum L., Spinacia oleracea L., Lactuca sativa L., and Brassica oleracea L. PMID:24250566

  7. Study on polarities of methylphenylpolysiloxanes in gas chromatography

    International Nuclear Information System (INIS)

    When studying the correlations between molecular structure and retention parameters in alcohols, alcohol benzoyl derivatives and carbonyl 2,4-dinitrophe nyl hydrazones some anomalies probably due to polarities of methylphenylpolysiloxane stationary phases have been observed. (Author) 31 refs

  8. SYNTHESIS, COMPUTATIONAL STUDY AND PRELIMINARY PHARMACOLOGICAL EVALUATION OF 2-[4-(2-CHLOROBENZYL/BENZOYL SUBSTITUTED PIPERAZIN-1-YL]-N-PHENYLACETAMIDE: POTENTIAL ANTIPSYCHOTICS

    Directory of Open Access Journals (Sweden)

    Tomar Amita

    2011-06-01

    Full Text Available Benzyl and benzoyl substituted acetamides have been synthesized and evaluated as potential antipsychotic agents. The target compounds (4a-b were prepared by reaction of substituted anilines with chloroacetylchloride which further treated with 2-chlorobenzyl or 2-chlorobenzoyl piperazine in presence of potassium carbonate and potassium iodide as catalyst in acetonitrile. The structures of the target compounds (4a-b were characterized on the basis of their M.P., TLC, IR and 1H-NMR data. Computational studies of target compounds (4a-b were carried out by using software programs. The target compounds showed good similarity with respect to standard drugs. The target compounds (4a-b showed inhibition of 5-HTP induced head twitches behavior and low induction of catalepsy in mice.

  9. Synthesis, Structure Characterization, and Cu2+ Recognition of 3-{[3-(Phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Aryl diketo acid derivatives are one of the most promising HIV-1 integrase(IN) inhibitors. With a view to substitute the critical diketo acid pharmacophore with the diketo benzimidazole unit, the coupling reaction of compound 4 with o -phenylenediamine was carried out. However, the reaction product, compound 5, was confirmed to be 3-{[3-(phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one rather than the2-benzimidazole derivative by using X-ray diffraction. Owing to its low solubility in water, the evaluation of the anti-HIV IN activity of the synthesized compound 5 could not be carried out. Consequently, the ion-binding properties of compound 5 in the absence of HIV-1 IN were investigated with UV-Vis spectroscopy in organic solvents. The results show that such a compound can selectively recognize Cu2+ .

  10. Mixed-ligand chelate extraction of trivalent lanthanides and actinides with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 and dihexyl-n, n-diethylcarbamoylmethyl phosphonate

    International Nuclear Information System (INIS)

    Mixed-ligand chelate extraction of trivalent lanthanides such as La, Eu and Lu and a trivalent actinide, Am into xylene with mixtures of 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP) and dihexyl-N, N-diathylcarbamoylmethylphosphonate (CMP) has been studied by tracer techniques. These trivalent metal ions are found to be extracted from 0.01 mol/dm3 chloroacetate buffer solutions as M(PMBP)3 x HPMBP type self adducts with HPMBP alone and in the presence of CMP as M(PMBP)3 x CMP (where M= La, Eu, Lu and Am) into the organic phase. The equilibrium constants of the above species are deduced by non-linear regression analysis. The synergistic constants of trivalent lanthanides do not increase monotonically with atomic number but have a maximum at Eu and that of Am was found to lie between that of La and Eu. (author). 12 refs., 3 figs., 3 tabs

  11. An efficient PEGylated liposomal nanocarrier containing cell-penetrating peptide and pH-sensitive hydrazone bond for enhancing tumor-targeted drug delivery

    Directory of Open Access Journals (Sweden)

    Ding Y

    2015-10-01

    Full Text Available Yuan Ding,1,* Dan Sun,1,* Gui-Ling Wang,1 Hong-Ge Yang,1 Hai-Feng Xu,1 Jian-Hua Chen,2 Ying Xie,1,3 Zhi-Qiang Wang4 1Beijing Key Laboratory of Molecular Pharmaceutics and New Drug Delivery Systems, School of Pharmaceutical Sciences, Peking University, Beijing, 2School of Medicine, Jianghan University, Wuhan, 3State Key Laboratory of Natural and Biomimetic Drugs, Peking University, Beijing, People’s Republic of China; 4Department of Chemistry and Biochemistry, Kent State University Geauga, Burton, OH, USA *These authors contributed equally to this work Abstract: Cell-penetrating peptides (CPPs as small molecular transporters with abilities of cell penetrating, internalization, and endosomal escape have potential prospect in drug delivery systems. However, a bottleneck hampering their application is the poor specificity for cells. By utilizing the function of hydration shell of polyethylene glycol (PEG and acid sensitivity of hydrazone bond, we constructed a kind of CPP-modified pH-sensitive PEGylated liposomes (CPPL to improve the selectivity of these peptides for tumor targeting. In CPPL, CPP was directly attached to liposome surfaces via coupling with stearate (STR to avoid the hindrance of PEG as a linker on the penetrating efficiency of CPP. A PEG derivative by conjugating PEG with STR via acid-degradable hydrazone bond (PEG2000-Hz-STR, PHS was synthesized. High-performance liquid chromatography and flow cytometry demonstrated that PHS was stable at normal neutral conditions and PEG could be completely cleaved from liposome surface to expose CPP under acidic environments in tumor. An optimal CPP density on liposomes was screened to guaranty a maximum targeting efficiency on tumor cells as well as not being captured by normal cells that consequently lead to a long circulation in blood. In vitro and in vivo studies indicated, in 4 mol% CPP of lipid modified system, that CPP exerted higher efficiency on internalizing the liposomes into

  12. Synthesis, Characterization, and Anti-Cancer Activity of Some New N′-(2-Oxoindolin-3-ylidene-2-propylpentane hydrazide-hydrazones Derivatives

    Directory of Open Access Journals (Sweden)

    Ayman El-Faham

    2015-08-01

    Full Text Available Eight novel N′-(2-oxoindolin-3-ylidene-2-propylpentane hydrazide-hydrazone derivatives 4a–h were synthesized and fully characterized by IR, NMR (1H-NMR and 13C-NMR, elemental analysis, and X-ray crystallography. The cyto-toxicity and in vitro anti-cancer evaluation of the prepared compounds have been assessed against two different human tumour cell lines including human liver (HepG2 and leukaemia (Jurkat, as well as in normal cell lines derived from human embryonic kidney (HEK293 using MTT assay. The compounds 3e, 3f, 4a, 4c, and 4e revealed promising anti-cancer activities in tested human tumour cells lines (IC50 values between 3 and 7 μM as compared to the known anti-cancer drug 5-Fluorouracil (IC50 32–50 μM. Among the tested compounds, 4a showed specificity against leukaemia (Jurkat cells, with an IC50 value of 3.14 μM, but this compound was inactive in liver cancer and normal cell lines.

  13. Mono- and binuclear copper(II) complexes of new hydrazone ligands derived from 4,6-diacetylresorcinol: Synthesis, spectral studies and antimicrobial activity

    Science.gov (United States)

    Shebl, Magdy; El-ghamry, Mosad A.; Khalil, Saied M. E.; Kishk, Mona A. A.

    Two new hydrazone ligands, H2L1 and H2L2, were synthesized by the condensation of 4,6-diacetylresorcinol with 3-hydrazino-5,6-diphenyl-1,2,4-triazine and isatin monohydrazone, respectively. The structures of the ligands were elucidated by elemental analyses, IR, 1H NMR, electronic and mass spectra. Reactions of the ligands with several copper(II) salts, including AcO-, NO3-, SO42-, Cl- and Br- afforded mono- and binuclear metal complexes. Also, the ligands were allowed to react with Cu(II) ion in the presence of a secondary ligand (L‧) [N,O-donor; 8-hydroxyquinoline, N,N-donor; 1,10-phenanthroline or O,O-donor; benzoylacetone]. Characterization and structure elucidation of the prepared complexes were achieved by elemental and thermal analyses, IR, electronic, mass and ESR spectra as well as conductivity and magnetic susceptibility measurements. The ESR spin Hamiltonian parameters of some complexes were calculated. The spectroscopic data showed that the H2L1 ligand acts as a neutral or monobasic tridentate ligand while the H2L2 ligand acts as a bis(monobasic tridentate) ligand. The coordination sites with the copper(II) ion are phenolic oxygen, azomethine nitrogen and triazinic nitrogen (H2L1 ligand) or isatinic oxygen (H2L2 ligand). The metal complexes exhibited octahedral and square planar geometrical arrangements depending on the nature of the anion. The ligands and some metal complexes showed antimicrobial activity.

  14. Cellular Delivery of Doxorubicin via pH-Controlled Hydrazone Linkage Using Multifunctional Nano Vehicle Based on Poly(β-L-Malic Acid

    Directory of Open Access Journals (Sweden)

    Keith L. Black

    2012-09-01

    Full Text Available Doxorubicin (DOX is currently used in cancer chemotherapy to treat many tumors and shows improved delivery, reduced toxicity and higher treatment efficacy when being part of nanoscale delivery systems. However, a major drawback remains its toxicity to healthy tissue and the development of multi-drug resistance during prolonged treatment. This is why in our work we aimed to improve DOX delivery and reduce the toxicity by chemical conjugation with a new nanoplatform based on polymalic acid. For delivery into recipient cancer cells, DOX was conjugated via pH-sensitive hydrazone linkage along with polyethylene glycol (PEG to a biodegradable, non-toxic and non-immunogenic nanoconjugate platform: poly(β-L-malic acid (PMLA. DOX-nanoconjugates were found stable under physiological conditions and shown to successfully inhibit in vitro cancer cell growth of several invasive breast carcinoma cell lines such as MDA-MB-231 and MDA-MB- 468 and of primary glioma cell lines such as U87MG and U251.

  15. Effect of the protonophore carbonyl cyanide-p-trifluoromethoxyphenyl-hydrazon on the glutamate release from rat brain nerve terminals under altered gravity conditions.

    Science.gov (United States)

    Borisova, T.; Krisanova, N.

    L-glutamate acts within the mammalian central nervous system as the predominant excitatory neurotransmitter and as a potent neurotoxin The balance between these physiological and pathological actions of glutamate is thought to be kept in check by the rapid removal of the neurotransmitter from the synaptic cleft The majority of uptake is mediated by the high-affinity Na -dependent glutamate transporters Depolarization leads to stimulation of glutamate efflux mediated by reversal of the high-affinity glutamate transporters The effects of the protonophore carbonyl cyanide-p-trifluoromethoxyphenyl-hydrazon FCCP on the glutamate release from isolated nerve terminals rat brain synaptosomes were investigated in control and after centrifuge-induced hypergravity rats were rotated in a long-arm centrifuge at ten-G during one-hour period The treatment of synaptosomes with 1 mu M FCCP during 11 min resulted in the increase in L- 14 C glutamate release by 23 0 pm 2 3 of total accumulated synaptosomal label in control animals and 24 0 pm 2 3 animals subjected to hypergravity FCCP evoked release of L- 14 C glutamate from synaptosomes was not altered in animals exposed to hypergravity as compared to control Glutamate transport is of electrogenic nature and thus depends on the membrane potential The high-KCl stimulated L- 14 C glutamate release in Ca 2 -free media occurred due to reversal of the glutamate transporters Carrier --mediated release of L- 14 C glutamate 6 min slightly increased as a result of

  16. A novel method for speciation of Cr(III) and Cr(VI) and individual determination using Duolite C20 modified with active hydrazone

    International Nuclear Information System (INIS)

    Trivalent and hexavalent chromium have been successfully separated and estimated from different solutions using 1-(3,4-dihydroxybenzaldehyde)-2-acetylpyridiniumchloride hydrazone (DAPCH) loaded on Duolite C20 in batch and column modes. The obtained modified resin [DAPCH-Duolite C20] was identified by C, H and N analyses and infrared spectra. The presence of multi-active chelating sites gives the ability for DAPCH to bind more chromium, Cr(III) by forming stable complex and chromate by forming ion pair molecule [H2DAPCH-Duolite C20]2+[Cr2O7]2- (H2DAPCH-Duolite C20 is the protonated form in acidic medium). The extraction isotherms were measured at different pH. The pH was found to be the backbone for the separation procedure in which the Cr(VI) and Cr(III) ions are sorbed selectively from aqueous solution at pH 2 and 6, respectively. The sorbed ions can be eluted using different concentrations of HCl. The saturation sorption capacity (41.6 and 20.05 mg g-1), the preconcentration factor (150 and 200) and the detection limit (13.3 and 10.0 ppb) were calculated for Cr(III) and (VI). The loaded resin can be regenerated for at least 50 cycles. The utility of the modified resin was tested in aqueous samples and shows R.S.D. value of <4% reflecting its accuracy and reproducibility

  17. Reactivity Differences between [alpha, beta]-Unsaturated Carbonyls and Hydrazones Investigated by Experimental and Theoretical Electron Density and Electron Localizability Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Grabowsky, Simon; Weber, Manuela; Jayatilaka, Dylan; Chen, Yu-Sheng; Grabowski, Matthias T.; Brehme, Rainer; Hesse, Malte; Schirmeister, Tanja; Luger, Peter (UWA); (Wurzburg); (UC); (Berlin)

    2012-10-11

    It is still a challenge to predict a compound's reactivity from its ground-state electronic nature although Bader-type topological analyses of the electron density (ED) and electron localizability indicator (ELI) give detailed and useful information on electron concentration and electron-pair localization, respectively. Both ED and ELI can be obtained from theoretical calculations as well as high-resolution X-ray diffraction experiments. Besides ED and ELI descriptors, the delocalization index is used here; it is likewise derived from theoretical calculations as well as from experimental X-ray results, but in the latter case, demonstrated here for the first time. We investigate {alpha},{beta}-unsaturated carbonyl and hydrazone compounds because resonance exhibited by these compounds in the electronic ground-state determines their reactive behavior. The degree of resonance as well as the reactivity contrast are quantified with the electronic descriptors. Moreover, competitive mesomeric substituent effects are studied using the two biologically important compounds acrolein and acrylamide. The reactivity differences predicted from the analyses are in line with the known reactivity of these compounds in organic synthesis. Hence, the capability of the ED and ELI for rationalizing and predicting different and competing substituent effects with respect to reactivity is demonstrated.

  18. 1,3-Dimethyl-5-(3,4,5-tris(alkoxy)benzoyl) barbituric acid derivatives and their liquid crystalline difluoroboron complexes: Synthesis, characterization and comparative investigations of mesomorphic, thermotropic and thermo-morphologic properties

    Science.gov (United States)

    Giziroglu, Emrah; Nesrullajev, Arif; Orhan, Nil

    2014-01-01

    A series of 1,3-dimethyl-5-(3,4,5-tris(alkoxy)benzoyl) barbituric acid derivatives 1a-4a with various chain length were synthesized by our group for the first time through the addition of 1,3-dimethyl barbituric acid to 3,4,5-tris(alkoxy)benzoyl chloride at room temperature in presence of pyridine. For preparation of their difluoroboron complexes, the derivatives 1a-4a reacts with borontrifluoride in the presence of triethylamine affording 1b-4b in moderate yields. All derivatives and complexes have been fully characterized by MS, FT-IR and multinuclear NMR spectroscopy. We also explored their liquid crystal properties by using POM, OM, CTW and DSC techniques. The results show that 3b and 4b with longer alkyl chain are monomorphic mesogens and exhibited enantiotropic thermotropic liquid crystalline mesophases. Investigation of their mesomorphic, thermo-morphologic and thermotropic properties is presented in this work.

  19. Ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride as a novel matrix for rapid quantitative and qualitative determination of serum free fatty acids by matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yaping [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China); Wang, Yanmin [Department of Clinical Laboratory, Heze Municipal Hospital, Shandong (China); Guo, Shuai; Guo, Yumei; Liu, Hui [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China); Li, Zhili, E-mail: lizhili@ibms.pumc.edu.cn [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China)

    2013-09-10

    Graphical abstract: -- Highlights: •A novel MALDI matrix for the detection of serum free fatty acids is ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride. •Multiple point internal standard calibration curves were constructed for nine FFAs, respectively, with excellent correlation coefficients between 0.991 and 0.999. •The MALDI-MS approach was used to rapidly differentiate the patients with and without hyperglycemia and healthy controls. -- Abstract: The blood free fatty acids (FFAs), which provide energy to the cell and act as substrates in the synthesis of fats, lipoproteins, liposaccharides, and eicosanoids, involve in a number of important physiological processes. In the present study, matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR MS) with ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride (ATNEDC) as a novel MALDI matrix in a negative ion mode was employed to directly quantify serum FFAs. Multiple point internal standard calibration curves between the concentration ratios of individual fatty acids to internal standard (IS, C{sub 17:0}) versus their corresponding intensity ratios were constructed for C{sub 14:0}, C{sub 16:1}, C{sub 16:0}, C{sub 18:0}, C{sub 18:1}, C{sub 18:2}, C{sub 18:3}, C{sub 20:4}, and C{sub 22:6}, respectively, in their mixture, with correlation coefficients between 0.991 and 0.999 and limits of detection (LODs) between 0.2 and 5.4 μM, along with the linear dynamic range of more than two orders of magnitude. The results indicate that the multiple point internal standard calibration could reduce the impact of ion suppression and improve quantification accuracy in the MALDI mode. The quantitative results of nine FFAs from 339 serum samples, including 161 healthy controls, 118 patients with hyperglycemia and 60 patients without hyperglycemia show that FFAs levels in hyperglycemic patient sera are significantly higher than those in healthy

  20. Structure-Toxicity Relations of Some Substituted 2-BENZOYL-1H-INDENE-1,3(2H)-DIONE Rodenticides.

    Science.gov (United States)

    Opong-Mensah, Kofi

    Chemical control of rodents depends primarily on the use of poisoned baits. The need for more potent rodenticides arises out of the evolution of resistant strains in rodent populations. One novel and 5 known benzoylindandiones were synthesized by condensation of methyl aryl ketones with dimethyl phthalate. Novel TLC, HPLC, and GC methods were developed to assay the acylindandiones after characterization by MS, IR and FT-NMR spectroscopy. The n-octanol/water partition coefficient (log P), acid dissociation constants (pKa) and mouse LD(,50)s were determined experimentally. Quantum mechanical molecular descriptors, such as HOMO-LUMO energies, were generated using computer models. The structure-toxicity relations of the benzoylindandiones were developed using regression models and partial least squares analysis. LD(,50)s (mM/Kg) for male Sprague-Dawley mice by intraperitoneal injection for 2-benzoyl-1,3-indandione (1), 2-(4'-methoxybenzoyl)-1,3-indandione (2), 2-(3'-methylbenzoyl) -1,3-indandione (3), 2-(4'-methylbenzoyl)-1,3-indandione (4), 2-(4'-isopropylbenzoyl)-1,3-indandione (5), and 2 -diphenylacetyl-1,3-indandione (6) were (median, 95% confidence limits): 1, 0.038 (0.030-0.049); 2, 0.026 (0.021-0.037); 3, 0.083 (0.065-0.106); 4, 0.077 (0.060-0.098); 5, 0.096 (0.071-0.128); and 6, 0.048 (0.035-0.064); log P was (mean (+OR-) standard error): 1, 1.14 (+OR-) 0.03; 2, 1.37 (+OR -) 0.02; 3, 1.24 (+OR-) 0.04; 4, 1.31 (+OR-) 0.02; 5, 1.43 (+OR-) 0.03 and 6, 2.47 (+OR-) 0.03; the pKas were (mean (+OR-) standard error): 1, 3.08 (+OR-) 0.02; 2, 3.91 (+OR -) 0.01; 3, 2.63 (+OR-) 0.01; 4, 2.93 (+OR-) 0.02; 5, 3.91 (+OR-) 0.01; and 6, 3.31 (+OR-) 0.01. -Log (,10)LD(,50) of the 6 indandiones correlated highly with the mean of the C-13 NMR chemical shifts of the carbonyl carbons, but poorly with pKa, IR carbonyl stretching frequencies, HOMO, LUMO, Hammett sigma and log P. 2-Benzoyl-1,3-indandione and 2-(4'-methoxybenzoyl) -1,3-indandione were more potent rodenticides than

  1. Synthesis, spectral studies and antibacterial activity of Cu(II), Co(II) and Ni(II) complexes of 1-(2-hydroxyphenyl)-3-phenyl-2-propen-1-one, N2-[(3,5-dimethyl-1H-pyrazol-1-yl)methyl]hydrazone

    OpenAIRE

    PAULMONY THARMARAJ; DEIVASIGAMANI KODIMUNTHIRI; CLARENCE D. SHEELA; CHAPPANI S. SHANMUGA PRIYA

    2009-01-01

    A new series of Cu(II), Co(II) and Ni(II) complexes with the 1-(2-hydroxyphenyl)-3-phenyl-2-propen-1-one, N2-[(3,5-dimethyl-1H-pyrazol-1-yl)methyl]hydrazone ligand, C21H22N4O (LH), were synthesized by the reaction of 1-(2-hydroxyphenyl)-3-phenyl-2-propen-1-one, hydrazone with (3,5-dimethyl-1H-pyrazol-1-yl)methanol and characterized. The nature of the bonding and geometry of the complexes were deduced from elemental analysis, IR, electronic and 1H-NMR spectroscopy, and magnetic susceptibility ...

  2. Application of 3-methylbenzothiazolin-2-one hydrazone for the quantitative spectrophotometric determination of oxcarbazepine in pharmaceuticals with cerium(IV) and periodate

    Science.gov (United States)

    Rajendraprasad, N.; Basavaiah, K.; Vinay, K. B.

    2012-09-01

    Two simple, sensitive, selective, accurate, and cost-effective spectrophotometric methods are described for the assay of oxcarbazepine (OXC) in bulk drug and in tablets. The methods are based on an oxidative coupling reaction involving OXC, 3-methylbenzothiazolin-2-one hydrazone (MBTH), and cerium(IV) sulfate at pH 4.28 ± 0.07 (method A) or sodium periodate at pH > 4.0 (method B) to form an orange colored product with an absorption maximum at 450 nm. Under optimized experimental conditions, the calibration graphs are linear over the ranges of 4-80 and 2-32 μg/ml for methods A and B, respectively, with correlation coefficient (r) values of 0.9984 and 0.9976. The apparent molar absorptivity values are 3.13ṡ103 and 9.13ṡ103 l/molṡcm for methods A and B, respectively. The other optical characteristics such as Sandell's sensitivity, limits of detection (LOD) and quantification (LOQ) values are also reported. The accuracy and precision of the methods were evaluated based on intra-day and inter-day variations. The proposed methods were successfully applied to the determination of OXC in tablets: the results were comparable with the published data obtained using the reference method. The reaction stoichiometry of OXC with MBTH (1:1 in method A and 1:2 in method B) was also evaluated using the limiting logarithmic method, and a possible reaction pathway is presented for the both methods.

  3. Synthesis and structure characterization of a new aromatic hydrazone%一种新型芳香酰腙的合成与结构表征

    Institute of Scientific and Technical Information of China (English)

    唐小冬; 郑长征; 田晓雪

    2011-01-01

    The title compound of l-(4-methoxyphenyl) ethanone 4-chlorob-en2oyl hydrazone was synthesized by the reaction of 4-methoxyphenyl ethyl ketone and 4-chlorobenzoyl hydrazine. The structure of the compound was characterized by elemental analysis and X-ray diffraction. It was assigned to orthorhombic crystal sy-stem, space group Pca2(l),cell data:a=0. 850 7(5)nm,a =90°,6 =0.557 1 (3)nm,£ = 90°, c = 3.215 4(18)nm,y = 90°,V = 1.523 9(14)nm3,Z=4,F(000) =632,/?, =0.031 7 [/ >2sigma(/)] ,wR2 =0.089 6. CCDC is 826 435.%目标化合物1-(4-甲氧基苯基)乙酮4-氯苯甲酰腙,由4-甲氧基苯基乙酮和4-氯苯甲酰肼通过脱水缩合反应制得,通过元素分析和X射线单晶衍射对目标化合物进行结构表征.检测数据表明,该新型酰腙为正交晶系,空间群为Pca2(1),晶胞学数据为α=0.850 7(5)nm,α=90°,b=0.557 1 (3) nm,β=90 °,c=3.215 4(18)nm,y=90°,V=1.523 9(14)nm3,Z =4,F(000)=632,R1 =0.031 7 [I>2sigma(I)],wR2=0.089 6.CCDC为826 435.

  4. Synthesis and quantitative structure-activity relationship (QSAR) study of novel N-arylsulfonyl-3-acylindole arylcarbonyl hydrazone derivatives as nematicidal agents.

    Science.gov (United States)

    Che, Zhiping; Zhang, Shaoyong; Shao, Yonghua; Fan, Lingling; Xu, Hui; Yu, Xiang; Zhi, Xiaoyan; Yao, Xiaojun; Zhang, Rui

    2013-06-19

    In continuation of our program aimed at the discovery and development of natural-product-based pesticidal agents, 54 novel N-arylsulfonyl-3-acylindole arylcarbonyl hydrazone derivatives were prepared, and their structures were well characterized by ¹H NMR, ¹³C NMR, HRMS, ESI-MS, and mp. Their nematicidal activity was evaluated against that of the pine wood nematode, Bursaphelenchus xylophilus in vivo. Among all of the derivatives, especially V-12 and V-39 displayed the best promising nematicidal activity with LC₅₀ values of 1.0969 and 1.2632 mg/L, respectively. This suggested that introduction of R¹ and R² together as the electron-withdrawing substituents, R³ as the methyl group, and R⁴ as the phenyl with the electron-donating substituents could be taken into account for further preparation of these kinds of compounds as nematicidal agents. Six selected descriptors are a WHIM descriptor (E1m), two GETAWAY descriptors (R1m+ and R3m+), a Burden eigenvalues descriptor (BEHm8), and two edge-adjacency index descriptors (EEig05x and EEig13d). Quantitative structure-activity relationship (QSAR) studies demonstrated that the structural factors, such as molecular mass (a negative correlation with the bioactivity) and molecular polarity (a positive correlation with bioactivity), are likely to govern the nematicidal activities of these compounds. For this model, the correlation coefficient (R²(training set)), the leave-one-out cross-validation correlation coefficient (Q²(LOO)), and the 7-fold cross-validation correlation coefficient (Q²(7-fold)) were 0.791, 0.701, and 0.715, respectively. The external cross-validation correlation coefficient (Q²ext) and the root-mean-square error for the test set (RMSE(test set)) were 0.774 and 3.412, respectively. This study will pave the way for future design, structural modification, and development of indole derivatives as nematicidal agents. PMID:23738496

  5. 闭管消解-萘乙二胺分光光度法测定水中总氮%Determination of Total Nitrogen in Water by Closed Digestion N - (1 -Naphthyl)ethyle Chromogenic Reaction

    Institute of Scientific and Technical Information of China (English)

    赵洋甬; 赵建平; 黄绍荣; 肖国起

    2012-01-01

    This paper established a new method of determining total nitrogen in water through closed digestion N - ( 1 - Naphthyl) ethyle chromogenic reaction, and analyzed the effect of different conditions to resaults at the same time based on experiment . The results show that water samples should be digested at least 25 minutes, and then chromogenically reacted for 5 ~ 20 minutes between 10~25℃ and finally determined at 535nm. This new method is more sensitive compared with the standard method,and it can be uesd to analysis the total nitrogen in water or wastewater.%通过实验研究了一种采用闭管消解-萘乙二胺分光光度法测定水样中总氮的新方法,分析了不同测试条件对测定结果的影响.结果表明:方法最佳消解时间为25min,宜选用535nm为实验波长,在10~25℃下显色5~ 20min完成测定.与标准方法比较,该方法具有灵敏度高、测定时间短的优点,可用于环境监测中水和废水的总氮分析.

  6. Photo-Fries rearrangements of 1-naphthyl (R-2-phenylpropanoate in poly(vinyl acetate and ethyl acetate: influence of medium polarity and polymer relaxation on motions of singlet radical pairs

    Directory of Open Access Journals (Sweden)

    Xu Jinqi

    2006-01-01

    Full Text Available Both the regio- and stereo-chemistries of the photoreactions of 1-naphthyl (R-2-phenylpropanoate have been investigated in poly(vinyl acetate films in their glassy (at 5masculineC and melted (at 50masculineC states and in ethyl acetate. These results are compared with those from irradiations in polyethylene films and in n-hexane. The regioselectivity of the intermediate 1-naphthoxy/(R-2-phenylpropanoyl radical pair combinations is much higher in both the melt and glassy states of poly(vinyl acetate films than that in the melt state of completely amorphous polyethylene films, but the stereoselectivity of intermediate prochiral 1-naphthoxy/1-phenylethyl radical pair combinations is much lower in poly(vinyl acetate. The results emphasize the need to control the ratio between the rates of radical tumbling and translation, as well as the ratio between the rates of in-cage motions and cage-escape, if high stereo- and regio-selectivities of combination products are to be achieved. A mechanistic picture of how the radicals of the intermediate pairs are affected by and interact with the various media is advanced.

  7. Sensitive quantitation of polyamines in plant foods by ultrasound-assisted benzoylation and dispersive liquid-liquid microextraction with the aid of experimental designs.

    Science.gov (United States)

    Pinto, Edgar; Melo, Armindo; Ferreira, Isabel M P L V O

    2014-05-14

    A new method involving ultrasound-assisted benzoylation and dispersive liquid-liquid microextraction was optimized with the aid of chemometrics for the extraction, cleanup, and determination of polyamines in plant foods. Putrescine, cadaverine, spermidine, and spermine were derivatized with 3,5-dinitrobenzoyl chloride and extracted by dispersive liquid-liquid microextraction using acetonitrile and carbon tetrachloride as dispersive and extraction solvents, respectively. Two-level full factorial design and central composite design were applied to select the most appropriate derivatization and extraction conditions. The developed method was linear in the 0.5-10.0 mg/L range, with a R(2) ≥ 0.9989. Intra- and interday precisions ranged from 0.8 to 6.9% and from 3.0 to 10.3%, respectively, and the limit of detection ranged between 0.018 and 0.042 μg/g of fresh weight. This method was applied to the analyses of six different types of plant foods, presenting recoveries between 81.7 and 114.2%. The method is inexpensive, versatile, simple, and sensitive. PMID:24773181

  8. Investigation of the formation of benzoyl peroxide, benzoic anhydride, and other potential aerosol products from gas-phase reactions of benzoylperoxy radicals

    Science.gov (United States)

    Strollo, Christen M.; Ziemann, Paul J.

    2016-04-01

    The secondary organic aerosol (SOA) products of the reaction of benzaldehyde with Cl atoms and with OH radicals in air in the absence of NOx were investigated in an environmental chamber in order to better understand the possible role of organic peroxy radical self-reactions in SOA formation. SOA products and authentic standards were analyzed using mass spectrometry and liquid chromatography, and results show that the yields of benzoyl peroxide (C6H5C(O)OO(O)CC6H5) and benzoic anhydride (C6H5C(O)O(O)CC6H5), two potential products from the gas-phase self-reaction of benzoylperoxy radicals (C6H5C(O)OO·), were less than 0.1%. This is in contrast to results of recent studies that have shown that the gas-phase self-reactions of β-nitrooxyperoxy radicals formed from reactions of isoprene with NO3 radicals form dialkyl peroxides that contribute significantly to gas-phase and SOA products. Such reactions have also been proposed to explain the gas-phase formation of extremely low volatility dimers from autooxidation of terpenes. The results obtained here indicate that, at least for benzoylperoxy radicals, the self-reactions form only benzoyloxy radicals. Analyses of SOA composition and volatility were inconclusive, but it appears that the SOA may consist primarily of oligomers formed through heterogeneous/multiphase reactions possibly involving some combination of phenol, benzaldehyde, benzoic acid, and peroxybenzoic acid.

  9. Determination of rhenium content in molybdenite by ICP-MS after separation of the major matrix by solvent extraction with N-benzoyl-N-phenylhydroxalamine.

    Science.gov (United States)

    Li, Jie; Zhong, Li-feng; Tu, Xiang-lin; Liang, Xi-rong; Xu, Ji-feng

    2010-05-15

    A simple and rapid analytical method for determining the concentration of rhenium in molybdenite for Re-Os dating was developed. The method used isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS) after the removal of major matrix elements (e.g., Mo, Fe, and W) from Re by solvent extraction with N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform solution. The effect on extraction efficiency of parameters such as pH (HCl concentration), BPHA concentration, and extraction time were also assessed. Under the optimal experimental conditions, the validity of the separation method was accessed by measuring (187)Re/(185)Re values for a molybdenite reference material (JDC). The obtained values were in good agreement with previously measured values of the Re standard. The proposed method was applied to replicate Re-Os dating of JDC and seven samples of molybdenite from the Yuanzhuding large Cu-Mo porphyry deposit. The results demonstrate good precision and accuracy for the proposed method. The advantages of the method (i.e., simplicity, efficiency, short analysis time, and low cost) make it suitable for routine analysis. PMID:20298878

  10. Synergistic solvent extraction of trivalent lanthanides and actinide by mixtures of 1-phenyl-3-methyl-4-benzoyl-pyrazalone-5 and neutral oxo-donors

    International Nuclear Information System (INIS)

    The synergistic solvent extraction of trivalent lanthanides such as La, Eu and Lu and a trivalent actinide, Am, has been studied with mixtures of 1-phenyl-3-methyl-4-benzoyl-pyrazalone-5 (HPMBP) and bis(2-ethylhexyl) sulphoxide (B2EHSO) or octyl (phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) in xylene. The extraction data have been analysed by both graphical and theoretical methods by taking into account aqueous phase speciation and all plausible complexes extracted into the organic phase. With HPMBP alone all the trivalent metal ions form M(PMBP)3 - HPMBP type self adducts. With B2EHSO as a neutral donor, the synergistic adduct species are M(PMBP)3 - B2EHSO and M(PMBP)3 - 2 B2EHSO (where M = La, Eu, Lu and Am), whereas with CMPO as a neutral donor the only complex extracted into the organic phase is M(PMBP)3 - CMPO. The synergistic extraction constants of the above species which were deduced by non-linear regression analysis are found to increase monotonically with decreasing ionic radii of these metal ions. 27 refs., 5 figs., 4 tabs

  11. Enhanced solubility and antibacterial activity of lipophilic fluoro-substituted N-benzoyl-2-aminobenzothiazoles by complexation with β-cyclodextrins.

    Science.gov (United States)

    Trapani, A; De Laurentis, N; Armenise, D; Carrieri, A; Defrenza, I; Rosato, A; Mandracchia, D; Tripodo, G; Salomone, A; Capriati, V; Franchini, C; Corbo, F

    2016-01-30

    Some lipophilic fluoro-substituted N-benzoyl-2-aminobenzothiazole antibacterial agents have been evaluated for their activity in the presence of cyclodextrins (CDs) containing aqueous solutions where CDs are adopted as solubilizing excipients for improving the poor water solubility of these compounds. For such purpose both the natural β-CD and one of FDA/EMA approved CDs for parenteral use (i.e. HP-β-CD) have been employed. The solubility rank order observed was accounted for by thermal analysis (Differential Scanning Calorimetry) and FT-IR spectroscopy. The most promising compound was subjected to further NMR spectroscopic studies and molecular modelling simulations to verify the interactions between the guest molecule and the CD cavity. The assessment of the antibacterial activity of such compounds against selected Gram positive and Gram negative bacterial strains clearly showed that their antimicrobial effectiveness may, quite in all instances, be positively affected by complexation with β-CD and HP-β-CD. These results, which are in some ways in contrast with those already reported in the literature, are herein discussed on the basis of plausible mechanisms. Moreover, this investigation also reveals that the described methodology of complexing both lipophilic and hydrophilic antimicrobial agents with CDs may be an useful approach to enhance their effectiveness as well as a promising strategy to overcome even the microbial resistance problem. PMID:26611670

  12. Densities, Ultrasonic Speeds, Viscosities and Refractive Indices of Binary Mixtures of Benzene with Benzyl Alcohol,Benzonitrile, Benzoyl Chloride and Chlorobenzene at 303.15 K

    Institute of Scientific and Technical Information of China (English)

    ALI,A.; PANDEY,J.D.; SONI,N.K.; NAIN,A.K.; LAL,B.; CHAND,D.

    2005-01-01

    Densities, p, ultrasonic speeds, u, viscosities, η, and refractive indices, n, of pure benzene, benzyl alcohol (BA),benzonitrile (BN), benzoyl chloride (BC), chlorobenzene (CB) and their thirty six binary mixtures, with benzene as common component, were measured at 303.15 K over the entire mole fraction range. From these experimental data the values of deviations in ultrasonic speed, Au, isentropic compressibility, Δks, excess acoustic impedance, ZE, deviation in viscosity, Δη, and excess Gibbs free energy of activation of viscous flow, G*E, and partial molar isentropic compressibility, Kφ,2 of BA, BN, BC and CB in benzene were computed. The variation of these derived functions with composition of the mixtures suggested the increased cohesion (molecular order) in the solution and that interaction (A-B)>(A-A) or (B-B). Moreover, theoretical prediction of ultrasonic speed, viscosity and refractive index of all the four binary mixtures was made on the basis of empirical and semi-empirical relations by using the experimental values of the pure components. Comparison of theoretical results with the experimental values was made in order to assess the suitability of these relations in reproducing the experimental values of u, η and n. Also, molecular radii of pure liquids and the average molecular radii of binary mixtures were evaluated using the corresponding refractive indices of pure liquids and binary mixtures. The average molecular radii of binary mixtures were found to be additive with respect to mole fraction of the pure component.

  13. Synthesis and Crystal Structure of a Manganese(Ⅱ) Complex with 2-(4'-Chlorine-benzoyl)-benzoic Acid and 1,10-Phenanthroline

    Institute of Scientific and Technical Information of China (English)

    WANG Qing-Wei; LI Xiu-Mei; MENG Qing-Long; LIU Bo; GAO Guang-Gang

    2009-01-01

    A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.154(5), b = 18.166(7), c =31.197(13) (A°), V = 6887(5) (A°)3, C80H48C14Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm3, μ(MoKa) =0.591 mm-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.

  14. The Melting Behavior and Thermal Stability of Green Poly(L-lactic acid) with N, N, N, N'-Tetra(benzoyl) Ethylene Diamine Tetraacetic Acid Dihydrazide

    International Nuclear Information System (INIS)

    The thermal properties of green poly(L-lactic acid) (PLLA) with N, N, N, N'-tetra(benzoyl) ethylene diamine tetraacetic acid dihydrazide (NA) at different conditions were investigated. The melting behavior of PLLA/NA sample after isothermal crystallization at 100 degree C showed that the low-temperature melting peak shifted to high temperature with increasing of crystallization time. However, the high-temperature melting peak did not show any change. Meantime, the melting enthalpy of cold crystallization was higher than that of hot crystallization, and the difference between cold crystallization and hot crystallization increased from 0.31 J/g to 0.89 J/g with increasing of crystallization time. Heating or cooling rate affected the melting behavior of PLLA, the low-temperature and high-temperature melting peak shifted to low temperature with increasing of rate, and the ratio of melting peak area between low-temperature melting peak and high-temperature melting peak decreased. Thermal stability of PLLA/NA indicated that PLLA/NA only exhibited one decomposition stage as decomposition of PLLA. (author)

  15. EFECTO DE HIDRAZONAS SOBRE AMASTIGOTES INTRACELULARES DE Leishmania panamensis Y UNA PROTEASA DE CISTEÍNA PARASITARIA EFFECT OF HYDRAZONES AGAINST INTRACELLULAR AMASTIGOTES OF Leishmania panamensis AND A PARASITIC CYSTEIN PROTEASE

    Directory of Open Access Journals (Sweden)

    Diana L. MUÑOZ

    2006-01-01

    Full Text Available En este trabajo se describe la síntesis de hidrazonas derivadas de cromano, tiocromano, alquil y aril hidrazonas, su actividad leishmanicida y su efecto sobre proteasas de cisteína de L. (V panamensis. Se sintetizan feniltiocromanos y bencil y naftil derivados; solamente las fenilhidrazonas muestran alguna actividad sobre amastigotes de Leishmnia (V panamensis. No se observa ningún efecto sobre una proteasa de cisteína del parásito lo que sugiere un mecanismo de acción diferente a la inhibición de esta enzima.In this paper, the synthesis of hydrazones derived from cromano, thiocroman, alkyl and aril hydrazones is described, as well as their leishmanicidal activity and their effect on cysteine proteases from L. (V panamensis. A series of novel phenylthiochromane and benzyl and naphtyl derivatives are synthesized and evaluated for their cytotoxic and antileishmanial activities. Their effect on parasite cysteine protease is also evaluated. Only phenylthiochromane derivatives display some activity against Leishmania (V panamensis but all compounds are inactive against parasitic cystein protease. These results may suggest a different mechanism of action for these compounds.

  16. Synthesis, characterisation, reactivity and in vitro antiamoebic activity of hydrazone based oxovanadium(IV), oxovanadium(V) and mu-bis(oxo)bis{oxovanadium(V)} complexes.

    Science.gov (United States)

    Maurya, Mannar R; Agarwal, Shalu; Abid, Mohammad; Azam, Amir; Bader, Cerstin; Ebel, Martin; Rehder, Dieter

    2006-02-21

    Binuclear, mu-bis(oxo)bis{oxovanadium(V)} complexes [(VOL)2(mu-O)2](2 and 7)(where HL are the hydrazones Hacpy-nah I or Hacpy-fah II; acpy = 2-acetylpyridine, nah = nicotinic acid hydrazide and fah = 2-furoic acid hydrazide) were prepared by the reaction of [VO(acac)2] and the ligands in methanol followed by aerial oxidation. The paramagnetic intermediate complexes [VO(acac)(acpy-nah)](1) and [VO(acac)(acpy-fah)](6) have also been isolated. Treatment of [VO(acac)(acpy-nah)] and [VO(acac)(acpy-fah)] with aqueous H2O2 yields the oxoperoxovanadium(V) complexes [VO(O2)(acpy-nah)](3) and [VO(O2)(acpy-fah)](8). In the presence of catechol (H2cat) or benzohydroxamic acid (H2bha), 1 and 6 give the mixed chelate complexes [VO(cat)L](HL =I: 4, HL =II: 9) or [VO(bha)L](HL =I: 5, HL =II: 10). Complexes 4, 5, 9 and 10 slowly convert to the corresponding oxo-mu-oxo species 2 and 7 in DMF solution. Ascorbic acid enhances this conversion under aerobic conditions, possibly through reduction of these complexes with concomitant removal of coordinated catecholate or benzohydroxamate. Acidification of 7 with HCl dissolved in methanol afforded a hydroxo(oxo) complex. The crystal and molecular structure of 2.1.5H2O has been determined, and the structure of 7 re-determined, by single crystal X-ray diffraction. Both of these binuclear complexes contain the uncommon asymmetrical {VO(mu-O)}2 diamond core. The in vitro tests of the antiamoebic activity of ligands I and II and their binuclear complexes 2 and 7 against the protozoan parasite Entamoeba histolytica show that the ligands have no amoebicidal activity while their vanadium complexes 2 and 7 display more effective amoebicidal activity than the most commonly used drug metronidazole (IC50 values are 1.68 and 0.45 microM, respectively vs 1.81 microM for metronidazole). Complexes 2 and 7 catalyse the oxidation of styrene and ethyl benzene effectively. Oxidation of styrene, using H2O2 as an oxidant, gives styrene epoxide, 2

  17. Vanadium complexes having [VO]2+, [VO]3+ and [VO2]+ cores with hydrazones of 2,6-diformyl-4-methylphenol: synthesis, characterization, reactivity, and catalytic potential.

    Science.gov (United States)

    Maurya, Mannar R; Haldar, Chanchal; Kumar, Amit; Kuznetsov, Maxim L; Avecilla, Fernando; Costa Pessoa, João

    2013-09-01

    The Schiff bases H3dfmp(L)2 obtained by the condensation of 2,6-diformyl-4-methylphenol and hydrazones [L = isonicotinoylhydrazide (inh), nicotinoylhydrazide (nah) and benzoylhydrazide (bhz)] are prepared and characterized. By reaction of [V(IV)O(acac)2] and the H3dfmp(L)2 in methanol the V(IV)O-complexes [V(IV)O{Hdfmp(inh)2}(H2O)] (1), [V(IV)O{Hdfmp(nah)2}(H2O)] (2) and [V(IV)O{Hdfmp(bhz)2}(H2O)] (3) were obtained. Upon their aerial oxidation in methanol [V(V)O(OMe)(MeOH){Hdfmp(inh)2}] (4), [V(V)O(OMe)(MeOH){Hdfmp(nah)2}] (5) and [V(V)O(OMe)(MeOH){Hdfmp(bhz)2}] (6) were isolated. In the presence of KOH, oxidation of 1-3 results in the formation of [V(V)O2{H2dfmp(inh)2}]n·5H2O (7), K[V(V)O2{Hdfmp(nah)2}] (8) and K[V(V)O2{Hdfmp(bhz)2}] (9). All compounds are characterized in the solid state and in solution, namely by spectroscopic techniques (IR, UV-Vis, EPR, (1)H, (13)C and (51)V NMR), and DFT is also used to calculate the V(IV) hyperfine coupling constants of V(IV)-compounds and (51)V NMR chemical shifts of several V(V)-species and assign them to those formed in solution. Single crystal X-ray analysis of [V(V)O(OMe)(MeOH){Hdfmp(bhz)2}] (6) and [V(V)O2{H2dfmp(inh)2}]n·5H2O (7) confirm the coordination of the ligand in the dianionic (ONO(2-)) enolate tautomeric form, one of the hydrazide moieties remaining non-coordinated. In the case of 7 the free N(pyridine) atom of the inh moiety coordinates to the other vanadium center yielding a polynuclear complex in the solid state. It is also demonstrated that the V(V)O2-complexes are catalyst precursors in the oxidative bromination of styrene by H2O2, therefore acting as functional models of vanadium dependent haloperoxidases. Plausible intermediates involved in the catalytic process are established by UV-Vis, (51)V NMR and DFT studies. PMID:23680862

  18. Bismuth(III) complexes with 2-acetylpyridine- and 2-benzoylpyridine-derived hydrazones: Antimicrobial and cytotoxic activities and effects on the clonogenic survival of human solid tumor cells.

    Science.gov (United States)

    Ferreira, Isabella P; Piló, Elisa D L; Recio-Despaigne, Angel A; Da Silva, Jeferson G; Ramos, Jonas P; Marques, Lucas B; Prazeres, Pedro H D M; Takahashi, Jacqueline A; Souza-Fagundes, Elaine M; Rocha, Willian; Beraldo, Heloisa

    2016-07-01

    Complexes [Bi(2AcPh)Cl2]·0.5H2O (1), [Bi(2AcpClPh)Cl2] (2), [Bi(2AcpNO2Ph)Cl2] (3), [Bi(2AcpOHPh)Cl2]·2H2O (4), [Bi(H2BzPh)Cl3]·2H2O (5), [Bi(H2BzpClPh)Cl3] (6), [Bi(2BzpNO2Ph)Cl2]·2H2O (7) and [Bi(H2BzpOHPh)Cl3]·2H2O (8) were obtained with 2-acetylpyridine phenylhydrazone (H2AcPh), its -para-chloro-phenyl- (H2AcpClPh), -para-nitro-phenyl (H2AcpNO2Ph) and -para-hydroxy-phenyl (H2AcpOHPh) derivatives, as well as with the 2-benzoylpyridine phenylhydrazone analogues (H2BzPh, H2BzpClPh, H2BzpNO2Ph, H2BzpOHPh). Upon coordination to bismuth(III) antibacterial activity against Gram-positive and Gram-negative bacterial strains significantly improved except for complex (4). The cytotoxic effects of the compounds under study were evaluated on HL-60, Jurkat and THP-1 leukemia, and on MCF-7 and HCT-116 solid tumor cells, as well as on non-malignant Vero cells. In general, 2-acetylpyridine-derived hydrazones proved to be more potent and more selective as cytotoxic agents than the corresponding 2-benzoylpyridine-derived counterparts. Exposure of HCT-116 cells to H2AcpClPh, H2AcpNO2Ph and complex (3) led to 99% decrease of the clonogenic survival. The IC50 values of these compounds were three-fold smaller when cells were cultured in soft-agar (3D) than when cells were cultured in monolayer (2D), suggesting that they constitute interesting scaffolds, which should be considered in further studies aiming to develop new drug candidates for the treatment of colon cancer. PMID:27209169

  19. Separation of trace amounts of high-valence elements in nickel with extraction and back-extraction using N-benzoyl-N-phenylhydroxylamine

    International Nuclear Information System (INIS)

    The separation and determination of trace amounts of Ti, Zr, Mo, Sn and Hf in Ni were studied. After the sample was dissolved with nitric acid, Ti, Zr, Mo, Sn and Hf were separated from Ni by extracting into benzene with N-benzoyl-N-phenylhydroxylamine (BPA) and subsequently back-extracted into nitric acid for the determination by ICP-AES or ICP-MS. The recoveries of Ti, Zr, Mo, Sn and Hf were satisfactory throughout the extraction with 4.0x10-2 mol·dm-3 BPA in benzene from 1.0 mol·dm-3 nitric acid-0.1 mol·dm-3 trichloroacetic acid solution and the back-extraction with 60% nitric acid. The separation factors (SM = DM/DNi, D = distribution ratios) of Ti, Zr, Mo, Sn and Hf from Ni were 9.9x103 for Ti, 3.2x104 for Zr, 3.2x104 for Mo, 1.3x103 for Sn and 4.0x104 for Hf. The recoveries of Ti, Zr, Mo, Sn and Hf decreased somewhat with increasing the added amount of Ni. The detection limits by ICP-MS were found to be 0.031 μg·g-1 for Ti, 0.046 μg·g-1 for Zr, 0.014 μg·g-1 for Mo, 0.7 μg·g-1 for Sn and 0.006 μg·g-1 for Hf using 0.5 g of Ni sample. The proposed method was applied to analysis of the real sample. (author)

  20. Synthesis and photoluminescence properties of silver(I) complexes based on N-benzoyl-L-glutamic acid and N-donor ligands with different flexibility

    Science.gov (United States)

    Yan, Ming-Jie; Feng, Qi; Song, Hui-Hua

    2016-05-01

    By changing the N-donor ancillary ligand, three novel silver (I) complexes {[Ag(HbzgluO) (4,4‧-bipy)]·H2O}n (1), {[Ag2(HbzgluO)2 (bpe)2]·2H2O}n (2) and {[Ag(HbzgluO)(bpp)]·2H2O}n (3) (H2bzgluO = N-benzoyl-L-glutamic acid, 4,4‧-bipy = 4,4ˊ-bipyridine, bpe = 1,2-di(4-pyridyl)ethane, bpp = 1,3-di(4-pyridyl)propane) were synthesized. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectra, powder X-ray diffraction (PXRD), and thermogravimetric analyses (TGA). In this study, the N-donor ligands are changed from rigidity (4,4‧-bipy), quasi-flexibility (bpe) to flexibility (bpp), the structures of complexes also change. Complex 1 features a 1D chain structure which is further linked together to construct a 2D supramolecular structure through hydrogen bonds. Complex 2 is a 1D double-chains configuration which eventually forms a 3D supramolecular network via hydrogen bonding interactions. Whereas, complex 3 exhibits a 2D pleated grid structure which is linked by hydrogen bonding interactions into a 3D supramolecular network. The present observations demonstrate that the modulation of coordination polymers with different structures can accomplish by changing the spacer length of N-donor ligands. In addition, the solid-state circular dichroism (CD) spectra indicated that compound 2 exhibited negative cotton effect which originated from the chiral ligands H2bzgluO and the solid-state fluorescence spectra of the three complexes demonstrated the auxiliary ligands have influence on the photoluminescence properties of the complexes.

  1. Formation of a dinuclear copper(II) complex through the cleavage of CN bond of 1-benzoyl-3-(pyridin-2-yl)-1H-pyrazole

    International Nuclear Information System (INIS)

    A simple mononuclear octahedral copper(II) complex was attempted from the reaction of three moles of 1-benzoyl-3-(pyridin-2-yl)-1H-pyrazole and one mole of copper(II) perchlorate hexahydrate in methanol. However, the product of the reaction was confirmed to be a dinuclear copper(II) complex with μ-(3-(pyridin-2-yl)-pyrazolato) and 3-(pyridin-2-yl)-1H-pyrazole ligands attached to each of the Cu(II) centre atom. The copper(II) ion assisted the cleavage of the CbenzoylN bond afforded a 3-(pyridin-2-yl)-1H-pyrazole molecule. Deprotonation of the 3-(pyridin-2-yl)-1H-pyrazole gave a 3-(pyridin-2-yl)-pyrazolato, which subsequently reacted with the Cu(II) ion to give the (3-(pyridin-2-yl)-pyrazolato)(3-(pyridin-2-yl)-1H-pyrazole)Cu(II) product moiety. The structure of the dinuclear complex was confirmed by x-ray crystallography. The complex crystallized in a monoclinic crystal system with P2(1)/n space group and cell dimensions of a = 12.2029(8) Å, b = 11.4010(7) Å, c = 14.4052(9) Å and β = 102.414(2)°. The compound was further characterized by mass spectrometry, CHN elemental analysis, infrared and UV-visible spectroscopy and the results concurred with the x-ray structure. The presence of d-d transition at 671 nm (ε = 116 dm3 mol−1 cm−1) supports the presence of Cu(II) centres

  2. Metal complexes of the nanosized ligand N-benzoyl-N‧-(p-amino phenyl) thiourea: Synthesis, characterization, antimicrobial activity and the metal uptake capacity of its ligating resin

    Science.gov (United States)

    Elhusseiny, Amel F.; Eldissouky, Ali; Al-Hamza, Ahmed M.; Hassan, Hammed H. A. M.

    2015-11-01

    The new nanosized N-benzoyl-N‧-(p-amino phenyl) thiourea ligand H2L was synthesized by nanoprecipitation method. The [Cu (H2L)2 Cl]·2H2O, [Zn (H2L)2(OAc)2], [Cd (H2L)2Cl2] and [Hg (H2L)2Cl2] complexes were synthesized and characterized by various physicochemical methods. Results revealed that the ligand act as hypodentate and bonded to the metal ion via the sulfur atom forming mononuclear non-electrolyte diamagnetic complex. Magnetic moment results indicated a reduction of Cu (II) to Cu (I) during the coordination process. Thermal studies demonstrated variable stabilities of the complexes and [Zn (H2L)2(OAc)2] exhibited the highest thermal stability while [Hg (H2L)2Cl2] was volatile. The prepared compounds were screened against different pathogenic microorganisms. The ligand performed high antibacterial activity against certain bacterial strain compared to its complexes, and the standard bacteriocide in use. The ligand was successfully immobilized on modified Amberlite XAD-16 forming the hypodentate ligating resin PS-SO2-H2L. The new resin was characterized and the extent of metal adsorption reached maximum at pH 6.0 for Cu (II), Cd (II) and Ag (I), with an adsorption amount of 4.3, 4.0 and 3.7 mmol g-1 respectively. The nanosized H2L represents a new category of promising adsorbent that would have a practical impact on biological and water treatment applications.

  3. Radiosensitization by 2-benzoyl-3-phenyl-6,7-dichloroquinoxaline 1,4-dioxide under oxia and hypoxia in human colon cancer cells

    International Nuclear Information System (INIS)

    The sensitizing effects of 2-benzoyl-3-phenyl-6,7-dichloroquinoxaline 1,4-dioxide (DCQ) and ionizing radiation (IR) were determined in four colon cancer cells and in FHs74Int normal intestinal cells. Cell cycle modulation, TUNEL assay, clonogenic survival and DNA damage were examined under oxia or hypoxia. Effects on apoptotic molecules and on p-Akt and Cox-2 protein expression were investigated. The four cell lines responded differently to DCQ+IR; HT-29 cells were most resistant. Combination treatment caused significant increases in preG1 (apoptosis) in HCT-116, while G2/M arrest occurred in DLD-1. DCQ potentiated IR effects more so under hypoxia than oxia. Pre-exposure of DLD-1 to hypoxia induced 30% apoptosis, and G2/M arrest in oxia. The survival rate was 50% lower in DCQ+IR than DCQ alone and this rate further decreased under hypoxia. FHs74Int normal intestinal cells were more resistant to DCQ+IR than cancer cells.Greater ssDNA damage occurred in DLD-1 exposed to DCQ+IR under hypoxia than oxia. In oxia, p-Akt protein expression increased upon IR exposure and drug pre-treatment inhibited this increase. In contrast, in hypoxia, exposure to IR reduced p-Akt protein and DCQ restored its expression to the untreated control. Apoptosis induced in hypoxic DLD-1 cells was independent of p53-p21 modulation but was associated with an increase in Bax/Bcl-2 ratio and the inhibition of the Cox-2 protein. DCQ is a hypoxic cell radiosensitizer in DLD-1 human colon cancer cells

  4. Multicenter study for efficacy and safety evaluation of a fixeddose combination gel with adapalen 0.1% and benzoyl peroxide 2.5% (Epiduo® for the treatment of acne vulgaris in Brazilian population*

    Science.gov (United States)

    Sittart, José Alexandre de Souza; da Costa, Adilson; Mulinari-Brenner, Fabiane; Follador, Ivonise; Azulay-Abulafia, Luna; de Castro, Lia Cândida Miranda

    2015-01-01

    BACKGROUND The current options for the treatment of acne vulgaris present many mechanisms of action. For several times, dermatologists try topical agents combinations, looking for better results. OBJECTIVES To evaluate the efficacy, tolerability and safety of a topical, fixed-dose combination of adapalene 0.1% and benzoyl peroxide 2.5% gel for the treatment of acne vulgaris in the Brazilian population. METHODS This is a multicenter, open-label and interventionist study. Patients applied 1.0 g of the fixed-dose combination of adapalene 0.1% and benzoyl peroxide 2.5% gel on the face, once daily at bedtime, during 12 weeks. Lesions were counted in all of the appointments, and the degree of acne severity, overall improvement, tolerability and safety were evaluated in each visit. RESULTS From 79 recruited patients, 73 concluded the study. There was significant, fast and progressive reduction of non-inflammatory, inflammatory and total number of lesions. At the end of the study, 75.3% of patients had a reduction of >50% in non-inflammatory lesions, 69.9% in inflammatory lesions and 78.1% in total number of lesions. Of the 73 patients, 71.2% had good to excellent response and 87.6% had satisfactory to good response. In the first week of treatment, erythema, burning, scaling and dryness of the skin were frequent complaints, but, from second week on, these signals and symptoms have reduced. CONCLUSION The fixed-dose combination of adapalene 0.1% and benzoyl peroxide 2.5% gel is effective, safe, well tolerated and apparently improves patient compliance with the treatment. PMID:27168522

  5. Adapalene 0.1% and benzoyl peroxide 2.5% as a fixed-dose combination gel is as well tolerated as the individual components alone in terms of cumulative irritancy.

    Science.gov (United States)

    Loesche, Christian; Pernin, Colette; Poncet, Michel

    2008-01-01

    International guidelines recommend the combination of retinoids (e.g. adapalene, tazarotene) and benzoyl peroxide for treating acne because of their complementary mechanisms of action. A new fixed-dose combination gel of adapalene 0.1% and benzoyl peroxide (BPO) 2.5% (adapalene/BPO*) is an effective acne treatment and offers the advantage of a once daily application. This paper reports the results of a cumulative irritancy study in healthy volunteers comparing adapalene/BPO to adapalene 0.1% and BPO 2.5% applied separately, BPO 10% gel, tazarotene 0.1% gel and the gel vehicle as a control.There was no significant difference between the mean cumulative irritation index (MCII) for adapalene/BPO and any test product except tazarotene 0.1% gel, which had a significantly greater MCII than all other test products (p < 0.05). This study showed that adapalene/BPO as a fixed-dose combination is as well tolerated as BPO 2.5% gel alone or adapalene 0.1% gel alone in terms of cumulative irritancy.*Epiduo, Galderma S.A. PMID:18693154

  6. Synthesis of Some N-Alkoxycarbonyl-N″-benzoyl-benzamidrazones(p-toluamidrazones) and 1,3,5-Trisubstituted 1,2,4-Triazole Derivatives from N-Benzoylimidates and their Antimicrobial and Anticancer Screening Studies

    Institute of Scientific and Technical Information of China (English)

    BEKIRCAN Olcay; KAHVECI Bahittin; OZGUMUS Osman Birol

    2007-01-01

    Some new N-alkoxycarbonyl-N″-benzoyl-benzamidrazones (p-toluamidrazones) 3a-3d,and 1,3,5-trisubstituted 1,2,4-triazole 4a-4h derivatives by starting from N-benzoylbenzimidates or N-benzoyl-p-toluimidates.The structures of compounds 3 and 4 were established on the basis of elemental analyses,IR,1H NMR,13C NMR and UV data.Antimicrobial experiments of the compounds performed by using agar-well diffusion and broth microdilution methods revealed that only compounds 3a-3d,4a and 4b showed inhibitory effect only on Candida albicans ATCC 60193.However,compound 4b had also specific antibacterial activity against Staphylococcus aureus ATCC 25923.The other compounds showed neither antifungal nor antibacterial activities.Compounds 3a,4a and 4b have been screened on three human tumor cell lines,breast cancer (MCF7),non small cell lung cancer (NCI-H460),and CNS cancer (SF-268) at the National Cancer Institute (NCI),USA,which were found to exhibit low antiproliferative activity.

  7. Determination of alkaline earth metal ions in solar salt by ion chromatography after solvent extraction with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone

    International Nuclear Information System (INIS)

    Ion chromatography was effectively applied to the determination of alkaline earth elements (Mg, Ca, Sr and Ba) in solar salt after extraction with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (HPMBP) into MIBK. The recommended procedure was as follows : the samples (20 ∼ 50 g) were dissolved in about 150 ml of water and the solution was filtered through filter paper into a 200-ml volumetric flask. Ten ml of the sample was pipetted into a centrifuge tube, 5 ml of NH3-NH4Cl buffer solution (pH 9.5), and 15 ml 0.05 M HPMBP-MIBK solution were added. The mixture was shaken vigorously for 30 min. After the phases were separated, an 8-ml portion of the organic phase was transferred into another tube and the alkaline earth elements were back-extracted with 8 ml of the 0.1 M hydrochloric acid. The aqueous phase (6 ml) was heated on a hot plate at 100 deg C in order to remove the dissolved MIBK in the phase. After cooling to room temperature, the solution was diluted to 25 ml with water. A 100 μl aliquot of the sample was analyzed by use of an ion chromatograph (Yokogawa Hokushin Electric Works, model IC 100) equipped with a precolumn (PCX 1, 50 mm x 4.6 mm i.d.) and a separation column (SCX 1, 250 mm x 4.6 mm i.d.) by using 2 mM ethylene diamine-4 mM tartaric acid as a mobile phase (2 ml/min). The detection limits (S/N = 2) were 1.5 ppb for Mg2+, 3.4 ppb for Ca2+, 20 ppb for Sr2+ and 50 ppb for Ba2+, respectively. Relative standard deviation (n = 7) was less than 6.3 % for the simultaneous determination of four elements. The recoveries of Mg2+, Ca2+, Sr2+ and Ba2+ by the proposed method were 100 ∼ 105, 95 ∼ 105, 97 ∼ 101 and 95 ∼ 101 %, respectively. (author)

  8. [7-(Fluoromethyl-2-naphthyl]methanol

    Directory of Open Access Journals (Sweden)

    Jane Bogdanov

    2014-02-01

    Full Text Available The title compound was synthesized from 2,7-bis(bromomethylnaphthalene via two step sequence-partial halogen exchange, followed by hydrolysis. The structure of this product was established by 1H-NMR, 13C-NMR, 19F-NMR, FT-IR spectroscopy and elemental analysis.

  9. Naphthyl azomesogens with lateral chloro groups†

    Indian Academy of Sciences (India)

    A K Prajapati; H M Pandya; N L Bonde

    2004-06-01

    A homologous series of azomesogens, 2"-[4-(4'--alkoxybenzoyloxy)-2-chlorophenylazo] naphthalenes, with lateral chloro groups was synthesised. All the homologues synthesized exhibit enantiotropic nematic mesophase. The mesomorphic properties of the present series are compared with other structurally related series to evaluate the effect of lateral chloro group and its position on mesomorphism.

  10. 离心沉淀气相色谱法测定面粉中过氧化苯甲酰含量的研究%Determination of Benzoyl Peroxide in Wheat Flour by Gas Chromatography after Precipitation by Centrifugation

    Institute of Scientific and Technical Information of China (English)

    应兴华; 徐霞; 朱智伟; 闵捷; 朱敏; 翟远建

    2009-01-01

    An analytical method of gas chromatography with flame ionization detection after precipitated by centrifugation was established for determination of benzoyl peroxide in wheat flour. The effects of different extraction time on the extraction efficiency and different calibration strategies for quantification were investigated, respectively. The benzoyl peroxide which was extracted from wheat flour with petroleum ether(60~90℃) was converted to benzoic acid in acidic condition, and then analyzed by gas chromatography with flame ionization detection. Recovery studies were performed at 0.06,0.18 and 0.30 g/kg fortification levels and the recoveries obtained ranging from 82.70% to 89.46% with relative standard deviations ranging from 3.77% to 6.93%. The method showed good linearity over the range assayed of 0.005~0.08 g/L and the detection limit was 2 mg/kg. The proposed method was suitable for determining benzoyl peroxide in wheat flour with high sensitivity, good accuracy and low-cost.%建立了离心沉淀,气相色谱氢火焰离子化检测器测定面粉中过氧化苯甲酰含量的方法.考察了不同提取时间和采用不同工作曲线对过氧化苯甲酰测定的影响.试样在石油醚中被冰乙酸还原成苯甲酸,经HP-5(30 m×0.25 mm×0.25 μm)毛细管气相色谱柱分离,氢火焰离子化检测器测定.方法的线性范围为0.005~0.08 g/L(r=0.9992),检出限(S/N=3)为2 mg/kg.在添标水平为0.06、0.18和0.30 g/kg时的平均回收率为82.70%~89.46%,相对标准偏差为3.77%~6.93%.该方法仪器设备简单,测定结果灵敏、准确,适合面粉中过氧化苯甲酰的测定.

  11. Synergistic extraction of U(VI) and Th(IV) from nitric acid with 4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-thione (HBMPPT) and tri-n-octylphosphine oxide (TOPO) in toluene

    International Nuclear Information System (INIS)

    The extractant HBMPPT (4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-thione) was synthesized from HBMPP. Its m.p. was 106-108 deg C. The synergistic extraction of U(VI) and Th(IV) from nitric acid solution by HBMPPT and TOPO in toluene was studied. The extraction ability of HBMPPT was not so high as that of its parent (HBMPP), but when a little tri-n-octylphophine oxide (TOPO) was added the ability to extract U(VI) and Th(IV) was seriously improved. The synergistic extracted complexes may be presented as UO2NO3 x BMPPT x TOPO and UO2(BMPPT)2 x TOPO for U(VI), and Th(NO3)3 x BMPPT x TOPO and Th(NO3)2(BMPPT)2 x TOPO for Th(IV) respectively. (author)

  12. Solvent extraction of lanthanide ions with 1-Phenyl-3-Methyl-4-Benzoyl-Pyrazolone-5 (HPMBP), 2. Extraction of Erbium(III), Ytterbium(III) and Lutetium(III) by HPMBP from aqueous-methanol solutions

    International Nuclear Information System (INIS)

    The solvent extraction of lanthanides(III)(Ln = Er, Yb, Lu) by 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HL) in carbon tetrachloride from aqueous-methanol phase was investigated. The equilibrium constants for the extraction from aqueous-50 % (ν/ν) methanol phase (Kex), two-phase stability constants of the complexes LnL3 (β3*) and stability constants of complexes LnL2+, LnL2+, LnL3(βn)(Ln = Yb, Lu) were calculated. It was confirmed that the addition of methanol to the aqueous phase causes a synergistic effect. The influence of methanol on the dissociation constant of HPMBP (Ka) and the distribution constant of HPMBP (pHL) between carbon tetrachloride and water-methanol solutions was investigated. (Authors)

  13. Solvent extraction of lanthanide ions with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP), III: extraction of gadolinium(III), terbium(III), dysprosium(III), holmium(III), and thulium(III) by HPMBP from aqueous solutions

    International Nuclear Information System (INIS)

    The solvent extraction behaviour of Gd(III), Tb(III), Dy(III), Ho(III), and Tm(III) has been investigated using 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP or HL) in carbon tetrachloride as the extractant. Depending on the concentration of HPMBP in the organic phase the chelates LnL3[Ln(III)=Gd, Tb, Dy, Ho, Tm] and adducts LnL3.HL[Ln(III)=Gd, Tb, Dy, Ho] were extracted. The extraction equilibrium constants (Kex3 or Kex4) for the formation of LnL3 or LnL3.HL and the two-phase stability constants of the chelates or adducts (β3x, β4x) have been evaluated. (authors)

  14. Studies on complexes of Cu(II), Ni(II), Co(II) and Ln(III) with 3-(α-benzoyl) benzylidenehydrazino-5, 6-diphenyl-1,2,4-triazine

    International Nuclear Information System (INIS)

    The synthesis, acid-base equilibria and metal-ion chelating tendencies of 3-(α-benzoyl) benzylidenehydrazino-5,6-diphenyl-1,2,4-triazine (BHT) are reported. From potentiometric equilibrium measurements of hydrogen ion concentration at 30degC and ionic strength 0.10 M KNO3, in 75% (v/v) dioxane-water medium, the values of the stability constants of BHT with transition and lanthanide(III) ions have been evaluated. Probable structures of metal chelates are inferred from electronic absorption spectra and infrared examination of solid complexes. The use of BHT as analytical reagent for the spectrophotometric determination of copper, nickel and cobalt has also been discussed. (author). 4 tabs., 3 figs., 20 refs

  15. (3-Benzoyl-1,7,7-trimethylbicyclo[2.2.1]heptan-2-olato-κ2O,Obis[2-(2-pyridylphenyl-κ2C1,N]iridium(III

    Directory of Open Access Journals (Sweden)

    Kaijun Luo

    2011-11-01

    Full Text Available The title compound, [Ir(C11H8N2(C17H19O2], has an octahedral coordination geometry around the IrIII atom, retaining the cis-C,C,trans–N,N chelate disposition of the two 2-phenylpyridine ligands. The chelate rings are nearly mutually perpendicular [the interplanar angles range from 85.48 (17 to 89.17 (19°]. The two 2-(2-pyridylphenyl ligands are approximately planar, with the plane of the phenyl ring being inclined to that of the pyridine ring by 2.3 (3 and 5.1 (3° in the two ligands. The interplanar angle between the phenyl ring in 3-benzoyl-camphor and the IrO2C3 chelate ring is 35.5 (2°.

  16. Solid State Structure and Solution Thermodynamics of Three-Centered Hydrogen Bonds (O∙∙∙H∙∙∙O Using N-(2-Benzoyl-phenyl Oxalyl Derivatives as Model Compounds

    Directory of Open Access Journals (Sweden)

    Carlos Z. Gómez-Castro

    2014-09-01

    Full Text Available Intramolecular hydrogen bond (HB formation was analyzed in the model compounds N-(2-benzoylphenylacetamide, N-(2-benzoylphenyloxalamate and N1,N2-bis(2-benzoylphenyloxalamide. The formation of three-center hydrogen bonds in oxalyl derivatives was demonstrated in the solid state by the X-ray diffraction analysis of the geometric parameters associated with the molecular structures. The solvent effect on the chemical shift of H6 [δH6(DMSO-d6–δH6(CDCl3] and Δδ(ΝΗ/ΔT measurements, in DMSO-d6 as solvent, have been used to establish the energetics associated with intramolecular hydrogen bonding. Two center intramolecular HB is not allowed in N-(2-benzoylphenylacetamide either in the solid state or in DMSO-d6 solution because of the unfavorable steric effects of the o-benzoyl group. The estimated ΔHº and ΔSº values for the hydrogen bonding disruption by DMSO-d6 of 28.3(0.1 kJ·mol−1 and 69.1(0.4 J·mol−1·K−1 for oxalamide, are in agreement with intramolecular three-center hydrogen bonding in solution. In the solid, the benzoyl group contributes to develop 1-D and 2-D crystal networks, through C–H∙∙∙A (A = O, π and dipolar C=O∙∙∙A (A = CO, π interactions, in oxalyl derivatives. To the best of our knowledge, this is the first example where three-center hydrogen bond is claimed to overcome steric constraints.

  17. A hydrazone Schiff base single crystal (E)-Methyl N(')-(3,4,5-trimethoxybenzylidene) hydrazine carboxylate: Physicochemical, in vitro investigation of antimicrobial activities and molecular docking with DNA gyrase protein.

    Science.gov (United States)

    Gomathi, G; Gopalakrishnan, R

    2016-07-01

    Hydrazone Schiff bases have been widely explored for their antimicrobial, anticancer, anticonvulsant properties. The aim of the present work is to investigate the spectroscopic, electrochemical, thermal properties, in vitro study of antimicrobial activity and molecular docking studies of the MBHC compound. Slow evaporation solution growth technique was used to grow the single crystal of the MBHC compound. Single crystal X-ray diffraction, FTIR and FT-Raman spectroscopic studies are performed and confirmed the grown MBHC compound. UV-Vis spectroscopy and electrochemical studies deduced the absorption region and HOMO-LUMO band gap value of the compound. Resazurin reduction assay method was utilized to perform antibacterial and antifungal studies which resulted in lesser effectiveness of the MBHC compound compared to the erythromycin and fluconazole tablets. Molecular docking of the MBHC compound with the DNA gyrase protein exhibited the good binding affinity with energy of -43.196kcal/mol and docking score of -6.266 and having good interaction with aminoacids - ASP81 and ARG84. PMID:27127037

  18. Comparative ligational, optical band gap and biological studies on Cr(III) and Fe(III) complexes of hydrazones derived from 2-hydrazinyl-2-oxo-N-phenylacetamide with both vanillin and O-vanillin

    Science.gov (United States)

    Yousef, T. A.; Abu El-Reash, G. M.; Attia, M. I.; El-Tabai, M. N.

    2015-09-01

    The Cr(III) and Fe(III) complexes of hydrazones derived from the condensation of 2-hydrazinyl-2-oxo-N-phenylacetamide with both vanillin and o-vanillin synthesized and characterized by different conventional physicochemical techniques. The kinetic and thermodynamic parameters for the different decomposition steps were calculated using Coats-Redfern and Horowitz-Metzger equations. The bond lengths, bond angles, HOMO, LUMO, dipole moment and binding energy calculated by DFT calculations. The optical band gap (Eg) values equal 3.28, 3.03, 3.58 and 3.57 eV for [Cr(HL1)Cl2(H2O)2](0.75H2O), [Cr(HL2)Cl2(H2O)](H2O), [Fe(HL1)Cl2(H2O)2](0.5H2O) and [Fe(HL2)2Cl(H2O)](3H2O) complexes, respectively. The antibacterial activities tested against Bacillus subtilis and Escherichia coli bacteria.

  19. Convenient one-pot synthesis of 2,5-anhydro-3,4,6-tri-O-benzoyl-D-(1-/sup 14/C)allononitrile, and its conversion to methyl 2-. beta. -D-ribofuranosyl-4-(2-/sup 14/C)selenazolecarboxylate

    Energy Technology Data Exchange (ETDEWEB)

    Woo, P.W.K.

    1988-10-01

    Reaction of 1-0-acetyl-2,3,5-tri-O-benzoyl-..beta..-D-ribofuranose with (/sup 14/C)cyanotrimethylsilane, generated in situ by reaction of potassium (/sup 14/C)cyanide and chloro-trimethylsilane in the presence of sodium iodide and 2,6-lutidine, gave 2,5-anhydro-3,4,6-tri-O-benzoyl-D-(1-/sup 14/C)allononitrile. Sequential reaction of the latter with hydrogen selenide, ethyl bromopyruvate, and methanolic sodium methoxide gave methyl ..beta..-D-ribofuranosyl-4-(2-/sup 14/C)selenazolcarboxylate, the penultimate precursor to (2-/sup 14/C)CI-935, or 2-..beta..-D-ribofuranosyl-4-(2-/sup 14/C)selenazolecarboxamide.

  20. Application of pyridine-2-carbaldehyde-2-(4-methyl-1,3-benzo thiazol-2-yl)hydrazone as a neutral ionophore in the construction of a novel Er(III) sensor

    Energy Technology Data Exchange (ETDEWEB)

    Ganjali, Mohammad Reza; Norouzi, Parviz [University of Tehran, Tehran (Iran, Islamic Republic of). Center of Excellence in Electrochemistry; Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of). Endocrine and Metabolism Research Center; E-mail: ganjali@khayam.ut.ac.ir; Rezapour, Morteza; Rasoolipour, Solmaz [University of Tehran, Tehran (Iran, Islamic Republic of). Center of Excellence in Electrochemistry; Adib, Mehdi [University of Tehran, Tehran (Iran, Islamic Republic of). University College of Science. Faculty of Chemistry

    2007-03-15

    We found that pyridine-2-carbaldehyde-2-(4-methyl-1,3-benzothiazol-2-yl) hydrazone (PCMHT) can be used as a suitable neutral ionophore for preparing an Er(III) membrane sensor with high selectivity. The optimum composition was found to be PCMHT-PVC-KTpClPB-BA with the ratios of 6.0:30.0:5.0:59.0, respectively. The Nernstian response was of 21.8 {+-} 0.5 mV decade{sup -1} of Er(III) activity, the linear range of the sensor was found to be relatively wide (from 1.0X10{sup -5} to 1.0 X10{sup -2} mol L{sup -1}). Its applicability pH range of 2.5-12.0 seems to make it suitable for analytical applications. The lower detection limit (LDL) of the sensor was 5.0 X10{sup -6} mol L{sup -1}. The excellent Er(III)-selectivity of the proposed sensor with regard to most common metal ions, and especially, lanthanide ions is another advantage. It was successfully used as an indicator electrode for titration of 25 mL of a 1.0 X 10{sup -4} mol L{sup -1} Er(III) ions with a 1.0 X 10{sup -}2 mol L{sup -1} EDTA. The proposed sensor was used for direct monitoring of Er(III) in binary mixtures and indirect determination of fluoride ions in two mouth wash preparations. (author)

  1. Synthesis, crystal structure analysis, spectral IR, NMR UV-Vis investigations, NBO and NLO of 2-benzoyl-N-(4-chlorophenyl)-3-oxo-3-phenylpropanamide with use of X-ray diffractions studies along with DFT calculations

    Science.gov (United States)

    Demir, Sibel; Sarioğlu, Ahmet Oral; Güler, Semih; Dege, Necmi; Sönmez, Mehmet

    2016-08-01

    The title compound, 2-benzoyl-N-(4-chlorophenyl)-3-oxo-3-phenylpropanamide compound (C22H16NO3Cl) has been synthesized and characterized by X-ray diffraction, IR, 1H and 13C NMR and UV-Vis spectra. Optimized geometrical structure, harmonic vibrational frequencies and chemical shifts were computed using hybrid-DFT (B3LYP and B3PW91) methods and 6-311G(d,p) as the basis set. The results of the optimized molecular structure are presented and compared with the experimental X-ray diffraction. The calculated optimized geometries, vibrational frequencies and 1H NMR chemical shift values are in strong agreement with experimentally measured values. UV-Vis spectrum of the title compound, was also recorded and the electronic properties, such as calculated energies, excitation energies, oscillator strengths, dipole moments and frontier orbital energies and band gap energies were computed with TDDFT-B3LYP methodolgy and using 6-311G(d,p) as the basis set. Furthermore, frontier molecular orbitals (FMO), molecular electrostatic potential (MEP), natural bond orbital (NBO) and non linear optical (NLO) properties were performed by using B3LYP/6-311G(d,p) level for the title compound.

  2. Binding of N-acetyl-N '-beta-D-glucopyranosyl urea and N-benzoyl-N '-beta-D-glucopyranosyl urea to glycogen phosphorylase b: kinetic and crystallographic studies.

    Science.gov (United States)

    Oikonomakos, Nikos G; Kosmopoulou, Magda; Zographos, Spyros E; Leonidas, Demetres D; Chrysina, Evangelia D; Somsák, László; Nagy, Veronika; Praly, Jean-Pierre; Docsa, Tibor; Tóth, Béla; Gergely, Pál

    2002-03-01

    Two substituted ureas of beta-D-glucose, N-acetyl-N'-beta-D-glucopyranosyl urea (Acurea) and N-benzoyl-N'-beta-D-glucopyranosyl urea (Bzurea), have been identified as inhibitors of glycogen phosphorylase, a potential target for therapeutic intervention in type 2 diabetes. To elucidate the structural basis of inhibition, we determined the structure of muscle glycogen phosphorylase b (GPb) complexed with the two compounds at 2.0 A and 1.8 A resolution, respectively. The structure of the GPb-Acurea complex reveals that the inhibitor can be accommodated in the catalytic site of T-state GPb with very little change in the tertiary structure. The glucopyranose moiety makes the standard hydrogen bonds and van der Waals contacts as observed in the GPb-glucose complex, while the acetyl urea moiety is in a favourable electrostatic environment and makes additional polar contacts with the protein. The structure of the GPb-Bzurea complex shows that Bzurea binds tightly at the catalytic site and induces substantial conformational changes in the vicinity of the catalytic site. In particular, the loop of the polypeptide chain containing residues 282-287 shifts 1.3-3.7 A (Calpha atoms) to accommodate Bzurea. Bzurea can also occupy the new allosteric site, some 33 A from the catalytic site, which is currently the target for the design of antidiabetic drugs. PMID:11895439

  3. When do efficacy outcomes in clinical trials correlate with clinical relevance? analysis of clindamycin phosphate 1.2%-benzoyl peroxide 3.75% gel in moderate to severe acne vulgaris.

    Science.gov (United States)

    Del Rosso, James Q

    2016-07-01

    Acne vulgaris (AV) is a common skin disease that is challenging to successfully treat due to its complex underlying pathophysiology and chronicity. Unrealistic expectations based on the desire for rapid and complete clearance or local tolerability reactions related to topical medications often lead to incomplete adherence with therapy, premature treatment cessation, and poor therapeutic outcomes. Despite stressing to patients the importance of compliance and the lag time of several weeks before visible improvement may be noted with treatments for AV, data on evaluation of the time taken to achieve a clinically meaningful improvement of AV that may be perceived by clinicians and patients are limited. Clindamycin phosphate 1.2%-benzoyl peroxide 3.75% (clindamycin-BP 3.75%) gel has been shown in pivotal trials to be effective and well tolerated in patients with moderate to severe AV. This article reviews a new concept referred to as time to onset of action (TOA), which is described in detail and illustrated using the pivotal trial data with clindamycin-BP 3.75% gel for treatment of AV. PMID:27529706

  4. Synthetic protease substrate n-benzoyl-L-argininyl-p-nitroanilide activates specific binding of [3H]estradiol to a protein in rat pancreas: relationship of structure to activity

    International Nuclear Information System (INIS)

    N-benzoyl-L-argininyl-p-nitroanilide (BAN), a synthetic substrate for trypsin-like proteolytic enzymes, is a potent activator of [3H]estradiol-binding to a protein present in rat pancreas. When partially purified, this protein is almost devoid of [3H]estradiol-binding activity in the absence of an endogenous accessory factor. BAN can mimic the natural coligand in this steroid binding reaction. The effect of BAN is specific since a number of derivatives of this substance are inactive or may even inhibit steroid binding. It is unlikely that BAN exerts this stimulatory action indirectly, possibly by preventing proteolytic inactivation of the [3H]estradiol-binding protein, since preincubation of the protein in the absence of BAN resulted neither in reduced rate, nor extent, of steroid binding following BAN addition. Also, a number of protease inhibitors had no effect on the binding reaction. Of those inhibitors tested, only antipain significantly enhanced binding of [3H]estradiol, but only about 20 percent as effectively as BAN. 13 references, 1 figure, 2 tables

  5. 合成4-苯甲酰基-1,7-庚二酸二甲酯的方法改进%Process Improvement on the Synthesis of 4-Benzoyl-heptanedioic Acid Dimethyl Ester

    Institute of Scientific and Technical Information of China (English)

    康从民; 李园园; 吕英涛

    2013-01-01

    采用改进方法,苯乙酮与丙烯酸甲酯缩合制得4-苯甲酰基-1,7-庚二酸二甲酯,其结构经1H NMR和MS确证.较适宜的反应条件为:苯乙酮50 mmol,n(丙烯酸甲酯)∶n(苯乙酮)=2.5∶1.O,无水环境下,以甲醇钠为催化剂,于50℃反应24h,收率12.8%.%4-Benzoyl-heptanedioic acid dimethyl ester was prepared by condensation of acetophenone with methyl acrylate by improve method. The structure was confirmed by 1H NMR and MS. The optimal reaction conditions at 50 ℃ for 24 h were as follows: acetophenone was 50 mmol, n( methyl acrylate) : n(acetophenone) was 2. 5 :1. 0, catalyst was MeONa in water-free. The yield was 12. 8% under the optimal conditions.

  6. End-to-End Thiocyanato-Bridged Helical Chain Polymer and Dichlorido-Bridged Copper(II) Complexes with a Hydrazone Ligand: Synthesis, Characterisation by Electron Paramagnetic Resonance and Variable-Temperature Magnetic Studies, and Inhibitory Effects on Human Colorectal Carcinoma Cells.

    Science.gov (United States)

    Das, Kuheli; Datta, Amitabha; Sinha, Chittaranjan; Huang, Jui-Hsien; Garribba, Eugenio; Hsiao, Ching-Sheng; Hsu, Chin-Lin

    2012-04-01

    The reactions of the tridentate hydrazone ligand, N'-[1-(pyridin-2-yl)ethylidene]acetohydrazide (HL), obtained by condensation of 2-acetylpyridine with acetic hyadrazide, with copper nitrate trihydrate in the presence of thiocyanate, or with CuCl2 produce two distinct coordination compounds, namely a one-dimensional helical coordination chain of [CuL(NCS)] n (1) units, and a doubly chlorido-bridged dinuclear complex [Cu2L2Cl2] (2) (where L=CH3C(O)=N-N=CCH3C5H4N). Single-crystal X-ray structural determination studies reveal that in complex 1, a deprotonated hydrazone ligand L(-) coordinates a copper(II) ion that is bridged to two neighbouring metal centres by SCN(-) anions, generating a one-dimensional helical coordination chain. In complex 2, two symmetry-related, adjacent copper(II) coordination entities are doubly chlorido-bridged, producing a dicopper entity with a Cu⋅⋅⋅Cu distance of 3.402 (1) Å. The two coordination compounds have been fully characterised by elemental analysis, spectroscopic techniques including IR, UV-vis and electron paramagnetic resonance, and variable-temperature magnetic studies. The biological effects of 1 and 2 on the viability of human colorectal carcinoma cells (COLO-205 and HT-29) were evaluated using an MTT assay, and the results indicate that these complexes induce a decrease in cell-population growth of human colorectal carcinoma cells with apoptosis. PMID:24551495

  7. Probing space charge effect on electroluminescence of indium tin oxide (ITO)/N,N′-di-[(1-naphthyl)-N,N′-diphenyl]-(1,1′-biphenyl)-4, 4′-diamine (α-NPD)/tris(8-hydroxy-quinolinato) aluminum (III) (Alq3)/Al diodes by time-resolved electric-field-induced optical second-harmonic generation measurement

    International Nuclear Information System (INIS)

    By using time-resolved electric-field-induced optical second-harmonic generation measurement, we studied the electroluminescence (EL) mechanism which is activated in double-layer organic light-emitting diodes (indium tin oxide/N,N′-di-[(1-naphthyl)-N,N′-diphenyl]-(1,1′-biphenyl)-4,4′-diamine (α-NPD)/tris(8-hydroxy-quinolinato) aluminum (III) (Alq3)/Al) in the high frequency region with application of AC square voltages at various duty-ratios. Results showed that holes were accumulated at the α-NPD/Alq3 interface in proportion to the duty-ratio, and corresponded well to the increasing EL enhancement at the high frequency. Our previous proposed model on the EL enhancement assisted by electron injection from the Al electrode in the presence of the space charge field was well confirmed. - Highlights: • We studied space charge (SC) effects in double-layer organic light emitting diodes. • The second-harmonic generation measurement was used to directly probe the SC field. • Space charge fields due to interfacial accumulated charge were verified. • We showed that SC electric fields contribute to electroluminescence emissions

  8. Probing space charge effect on electroluminescence of indium tin oxide (ITO)/N,N′-di-[(1-naphthyl)-N,N′-diphenyl]-(1,1′-biphenyl)-4, 4′-diamine (α-NPD)/tris(8-hydroxy-quinolinato) aluminum (III) (Alq{sub 3})/Al diodes by time-resolved electric-field-induced optical second-harmonic generation measurement

    Energy Technology Data Exchange (ETDEWEB)

    Sadakata, Atsuo; Osada, Kenshiro; Taguchi, Dai; Manaka, Takaaki; Iwamoto, Mitsumasa, E-mail: iwamoto@pe.titech.ac.jp

    2014-03-03

    By using time-resolved electric-field-induced optical second-harmonic generation measurement, we studied the electroluminescence (EL) mechanism which is activated in double-layer organic light-emitting diodes (indium tin oxide/N,N′-di-[(1-naphthyl)-N,N′-diphenyl]-(1,1′-biphenyl)-4,4′-diamine (α-NPD)/tris(8-hydroxy-quinolinato) aluminum (III) (Alq{sub 3})/Al) in the high frequency region with application of AC square voltages at various duty-ratios. Results showed that holes were accumulated at the α-NPD/Alq{sub 3} interface in proportion to the duty-ratio, and corresponded well to the increasing EL enhancement at the high frequency. Our previous proposed model on the EL enhancement assisted by electron injection from the Al electrode in the presence of the space charge field was well confirmed. - Highlights: • We studied space charge (SC) effects in double-layer organic light emitting diodes. • The second-harmonic generation measurement was used to directly probe the SC field. • Space charge fields due to interfacial accumulated charge were verified. • We showed that SC electric fields contribute to electroluminescence emissions.

  9. 苯亚甲基苯乙酮-4-氯苯甲酰腙的合成、晶体结勾及荧光性质%Synthesis, crystal structure and fluorescence properties of benzylidene acetophenone-4-chlorobenzoyl hydrazone

    Institute of Scientific and Technical Information of China (English)

    王亮; 刘娟; 郑长征; 任立娣

    2011-01-01

    由苯亚甲基苯乙酮和4-氯苯甲酰肼通过缩合反应,合成新的酰腙化合物苯亚甲基苯乙酮-4-氯苯甲酰腙,并培养成单晶( CCDC:848755).通过元素分析、红外光谱和X射线单晶衍射对其进行了结构表征.结果表明,该化合物为单斜晶系,空间群为P2(1)/n,晶胞学数据:a=0.913 4(6) nm,b=2.451 0(17) nm,c =0.948 9(7) nm,β=118.77.,V=1.862(2) nm3,Z=4,μ=0.218 mm-1,Dc=1.287 mg/m3,F(000) =752,R1 =0.072 2[I>2δ(I)],wR2=0.226 7(all data),GOF=0.968.荧光光谱表明,该化合物的荧光性能较好,可以作为一种潜在的光活性材料.%A new compound of benzylidene acetophenone-4-chlorobenzoyl hydrazone was synthesized through the condensation of benzylidene acetophenone and 4-chlorobenzoyl hydrazine, then it was developed into a single crystal (CCDC:848755). The compound was characterized by elemental analysis, IR and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to the monoclinic system with space group P2(1)/n, with α = 0. 913 4(6) nm,b =2. 451 0(17) nm, c =0.948 9(7) nm,β = 118.77°,V=1.862(2) nm3 ,Z =4, μ =0. 218 mm-1, Dc =1.287 mg/m3, F(000) =752,R, = 0.072 2[I>2δ(I)],wR2 =0.226 7(all data) ,GOF =0.968. Fluorescence spectra showed that the compound was a strong fluorescent substances can be used as a potential photoactive ma terials.

  10. Kinetic Study on Nucleophilic Displacement Reactions of Y-Substituted-Phenyl 2-Methylbenzoates with Cyclic Secondary Amines in Acetonitrile: Effects of Modification of 2-MeO in Benzoyl Moiety by 2-Me on Reactivity and Reaction Mechanism

    International Nuclear Information System (INIS)

    The second-order rate constants (kN) have been measured spectrophotometrically for nucleophilic substitution reactions of Y-substituted-phenyl 2-methylbenzoates (6a-e) with a series of cyclic secondary amines in MeCN at 25.0 ± 0.1 .deg. C. Comparison of the kN values for the reactions of 4-nitrophenyl 2-methylbenzoate (6d) with those reported previously for the corresponding reactions of 4-nitrophenyl 2-methoxybenzoate (5) reveals that 6d is significantly less reactive than 5, indicating that modification of 2-MeO in the benzoyl moiety of 5 by 2-Me (i. e., 5 → 6d) causes a significant decrease in reactivity. This supports our previous report that aminolysis of 5 proceeds through a six-membered cyclic intermediate, which is highly stabilized through intramolecular H-bonding interactions. The Brφnsted-type plot for the reactions of 6d with a series of cyclic secondary amines is linear with βnuc = 0.71, which appears to be a lower limit of βnuc for a stepwise mechanism with breakdown of an intermediate (T±) being rate-determining step (RDS). The Brφnsted-type plot for the reactions of 6a-e with piperidine is curved, i. e., the slope of Brφnsted-type plot (βlg) decreases from -1.05 to -0.41 as the leaving-group basicity decreases. The nonlinear Brφnsted-type plot has been taken as evidence for a stepwise mechanism with a change in RDS (e. g., from the k2 step to the k1 process as the leaving-group basicity decreases). Dissection of kN into the microscopic rate constants associated with the reactions of 6a-e with piperidine (e. g., k1 and k2/k-1 ratio) also supports the proposed mechanism

  11. Adapalene-benzoyl peroxide once-daily, fixed-dose combination gel for the treatment of acne vulgaris: a randomized, bilateral (split-face), dose-assessment study of cutaneous tolerability in healthy participants.

    Science.gov (United States)

    Andres, Philippe; Pernin, Colette; Poncet, Michel

    2008-03-01

    Combination therapy is an effective approach to simultaneously target multiple pathogenic factors of acne. International consensus guidelines recommend the use of topical retinoids and benzoyl peroxide (BPO) for acne treatment. These drugs are often prescribed as a free combination without any safety concern associated with antibiotic use. A 3-week, randomized, controlled, investigator-blinded, single-center, bilateral (split-face), dose-assessment study was conducted comparing the cutaneous tolerability of 2 adapalene-BPO fixed-dose combination products versus various concentrations of BPO monotherapy applied once daily. Sixty healthy participants were randomized to one of the following treatment groups: adapalene 0.1%-BPO 2.5% combination product versus BPO 2.5% monotherapy; adapalene 0.1%-BPO 2.5% combination product versus BPO 5% monotherapy; adapalene 0.1%-BPO 5% combination product versus BPO 5% monotherapy; and adapalene 0.1%-BPO 5% combination product versus BPO 10% monotherapy. Assessments included total sum score (TSS) of irritation signs/ symptoms (erythema, scaling/desquamation, dryness, pruritus, stinging/burning) averaged over all postbaseline visits, individual irritation signs/symptoms (worst score), and adverse events. The overall cutaneous tolerability profile of the adapalene 0.1%-BPO 2.5% combination product was better than the combination with BPO 5% and similar to BPO 2.5% or 5% monotherapy. The combination product with BPO 5% induced significantly more irritation than BPO 5% monotherapy (P < .001) or BPO 10% monotherapy (P = .001). In conclusion, the new fixed-dose adapalene 0.1%-BPO 2.5% combination product provided the best overall cutaneous tolerability profile relative to BPO monotherapy. PMID:18441854

  12. Synthesis, Characterization And Antitumor Activity Of Copper(II Complexes, [CuL2] [HL1-3=N,N-Diethyl-N'-(R-BenzoylThiourea (R=H, o-Cl and p-NO2

    Directory of Open Access Journals (Sweden)

    Evgenia Spodine

    2004-01-01

    Full Text Available The copper (II complexes (CuL2 were prepared by reaction of Cu(CH3COO2 with the corresponding derivatives of acylthioureas in a Cu:HL molar ratio of 1:2. Acylthiourea ligands, N,N-diethyl-N'-(R-benzoyl thiourea (HL1-3 [R=H, o-Cl and p-NO2] were synthesized in high yield (78-83% and characterized by elemental analysis, infrared spectroscopy, 1H and 13C NMR spectroscopy. The complexes CuL2 were characterized by elemental analysis, IR, FAB(+-MS, magnetic susceptibility measurements, EPR and cyclic voltammetry. The crystal structure of the complex Cu(L22 shows a nearly square-planar geometry with two deprotonated ligands (L coordinated to CuII through the oxygen and sulfur atoms in a cis arrangement. The antitumor activity of the copper(II complexes with acylthiourea ligands was evaluated in vitro against the mouse mammary adenocarcinoma TA3 cell line. These complexes exhibited much higher cytotoxic activity (IC50 values in the range of 3.9-6.9 μM than their corresponding ligands (40-240 μM, which indicates that the coordination of the chelate ligands around the CuII enhances the antitumor activity and, furthermore, this result confirmed that the participation of the nitro and chloro substituent groups in the complex activities is slightly relevant. The high accumulation of the complexes Cu(L22 and Cu(L32 in TA3 tumor cells and the much faster binding to cellular DNA than Cu(L12 are consistent with the in vitro cytotoxic activities found for these copper complexes.

  13. Study of chromatographic enantioseparation of the esters of N-dinitrobenzoyl (N-DNB) and N-benzoyl (N-B) alpha-amino acids on novel chiral stationary phases containing structurally matching N-DNB and N-B-alpha-AA amides in the chiral selector

    OpenAIRE

    Zafirova, Biljana; Landek, Goran; Kontrec, Darko; Šunjić, Vitomir; Vinković, Vladimir

    2004-01-01

    Enantioseparation ability and enantiopreference of chiral stationary phases CSP 1–CSP 3, containing a terminal N-3,5-dinitrobenzoyl (N-DNB) unit, and CSP 4, containing a terminal N-benzoyl (N-B) unit, are studied. Separation factors (α) for the two sets of test racemates (TR) that structurally match the chiral selector of these CSPs have been determined. The first set consists of seven N-DNB α-amino acid isopropylesters (TR 1A–TR 7A), and the second one of their N-B analogues (TR ...

  14. FIRST X-RAY CRYSTAL STRUCTURE OF A BIMETALLIC COMPLEX CONTAINING A p -COORDINATED HYDRAZONE: [(h 5-CpFe(h 6-p-MeOC6H4-NHN=CH-(h 5-C5H4Fe(h 5-Cp]+PF6

    Directory of Open Access Journals (Sweden)

    Carolina Manzur

    2001-12-01

    Full Text Available The dinuclear organometallic hydrazone [(h 5-CpFe(h 6-p-MeO-C6H4-NHN=CH-(h 5-C5H4Fe(h 5-Cp]+PF6- (Cp=C5H5 is stereoselectively prepared as its trans isomer by reacting the organometallic hydrazine precursor [(h 5-CpFe(h 6-p-MeO-C6H4-NHNH2]+PF6- with the ferrocenecarboxaldehyde. Its crystalline and molecular structure has been determined and consists of two iron(II sandwiches of the type [(h 5-CpFe(h 6-arene]+ and [(h 5-C5H4Fe(h 5-Cp], in anti position one with respect to the other, and linked by a zigzag hydrazonic spacerLa hidrazona organometálica dinuclear [(h 5-CpFe(h 6-p-MeO-C6H4-NHN=CH-(h 5-C5H4Fe(h 5-Cp]+PF6- es preparada estereoquímicamente como su isómero trans por reacción de la hidracina organometálica precursora [(h 5-CpFe(h 6-p-MeO-C6H4-NHNH2]+PF6- con ferrocencarboxaldehido. Se ha determinado su estructura cristalina y molecular que consiste en dos sanwiches de hierro(II del tipo [(h 5-CpFe(h 6-areno]+ y [(h 5-C5H4Fe(h 5-Cp] en posición anti uno respecto del otro, los que se encuentran enlazados por un espaciador hidrazónico en forma de zig-zag

  15. N-Benzoyl-N′-phenyl­urea

    OpenAIRE

    Okuniewski, Andrzej; Chojnacki, Jaroslaw; BECKER, Barbara

    2010-01-01

    In the title compound, C14H12N2O2, the mol­ecular conformation is determined by a strong intra­molecular N—H⋯O=C hydrogen bond. In the crystal, pairs of mol­ecules are connected by inter­molecular N—H⋯O=C hydrogen bonds, forming centrosymmetric dimers. No specific inter­actions between dimers could be found.

  16. (E-3-Anilino-2-benzoyl-3-(methylsulfanylacrylonitrile

    Directory of Open Access Journals (Sweden)

    Hatem A. Abdel-Aziz

    2012-04-01

    Full Text Available In the title acrylonitrile derivative, C17H14N2OS, the central aminoacrylaldehyde O=C—C=C—NH unit, wherein an intramolecular N—H...O hydrogen bond generates an S(6 ring motif, is approximately planar, with an r.m.s. deviation of 0.0234 (2 Å for the five non-H atoms. This plane makes dihedral angles of 41.04 (9 and 84.86 (10° with the two phenyl rings. The dihedral angle between the two phenyl rings is 54.82 (10°. An intramolecular C—H...N hydrogen bond is also present. In the crystal, weak C—H...π and π–π interactions, with a centroid–centroid distance of 3.8526 (14 Å, are observed.

  17. Formation of a dinuclear copper(II) complex through the cleavage of CN bond of 1-benzoyl-3-(pyridin-2-yl)-1H-pyrazole

    Energy Technology Data Exchange (ETDEWEB)

    Shardin, Rosidah; Pui, Law Kung; Yamin, Bohari M. [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, UKM 43600 Bangi, Selangor (Malaysia); Kassim, Mohammad B. [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, UKM 43600 Bangi, Selangor, Malaysia and Fuel Cell Institute, Universiti Kebangsaan Malaysia, UKM 43600 Bangi, Selangor (Malaysia)

    2014-09-03

    A simple mononuclear octahedral copper(II) complex was attempted from the reaction of three moles of 1-benzoyl-3-(pyridin-2-yl)-1H-pyrazole and one mole of copper(II) perchlorate hexahydrate in methanol. However, the product of the reaction was confirmed to be a dinuclear copper(II) complex with μ-(3-(pyridin-2-yl)-pyrazolato) and 3-(pyridin-2-yl)-1H-pyrazole ligands attached to each of the Cu(II) centre atom. The copper(II) ion assisted the cleavage of the C{sub benzoyl}N bond afforded a 3-(pyridin-2-yl)-1H-pyrazole molecule. Deprotonation of the 3-(pyridin-2-yl)-1H-pyrazole gave a 3-(pyridin-2-yl)-pyrazolato, which subsequently reacted with the Cu(II) ion to give the (3-(pyridin-2-yl)-pyrazolato)(3-(pyridin-2-yl)-1H-pyrazole)Cu(II) product moiety. The structure of the dinuclear complex was confirmed by x-ray crystallography. The complex crystallized in a monoclinic crystal system with P2(1)/n space group and cell dimensions of a = 12.2029(8) Å, b = 11.4010(7) Å, c = 14.4052(9) Å and β = 102.414(2)°. The compound was further characterized by mass spectrometry, CHN elemental analysis, infrared and UV-visible spectroscopy and the results concurred with the x-ray structure. The presence of d-d transition at 671 nm (ε = 116 dm{sup 3} mol{sup −1} cm{sup −1}) supports the presence of Cu(II) centres.

  18. 2-(2-Naphthyl-1,3-dioxane

    Directory of Open Access Journals (Sweden)

    Damien Thevenet

    2010-02-01

    Full Text Available The title compound, C14H14O2, crystallizes in the chiral monoclinic space group P21. This acetal is composed of a planar naphthalene ring with a 1,3-dioxane ring substituent, which has a chair conformation. In the crystal structure, symmetry-related molecules are connected via a weak C—H...O interaction to form a helical chain propagating in [010]. While there are no π–π stacking interactions present, there are weak C—H...π interactions involving the naphthalene aromatic rings, which link the helical chains to form a two-dimensional network in the (011 plane.

  19. SYNTHESIS OF NOVEL FURAN AND THEIR HYDRAZONES Synthese von neuartigen FURAN UND IHRE Hydrazone

    Directory of Open Access Journals (Sweden)

    Vijay V Dabholkar and Syed Sagir Ahmed

    2011-10-01

    Full Text Available β-Benzoylproponic acid (1 on lactonization reaction with excess of acetic anhydride, and few drops of concentrated sulfuric acid as a catalyst reviled 5-phenyl-furan-2(3H-ones (2. A mixture of 5-phenyl-furan-2(3H-ones with aromatic aldehydes, potassium hydroxide as a catalyst result to 2-Phenyl-4-benzylidene-5-hydrazinofuran-2-ene (3, which on further reaction with hydrazine hydrates yielded corresponding 5-hydrazine (4. This on condensation reaction with different aldehydes reviled final 2-Phenyl-4-benzylidene-5-benzylidinehydrazo-furan-2-ene (5. The structures of the compounds have been elucidated on the basis of spectral analysis.

  20. Eficácia da combinação tópica de peróxido de benzoíla 5% e clindamicina 1% para o tratamento da hipomelanose macular progressiva: um estudo randomizado, duplo-cego, placebo-controlado Efficacy of topical combination of benzoyl peroxide 5% and clindamycin 1% for the treatment of progressive macular hypomelanosis: a randomized, doubleblind, placebo-controlled trial

    Directory of Open Access Journals (Sweden)

    Jussamara Brito Santos

    2011-02-01

    Full Text Available FUNDAMENTOS: A hipomelanose macular progressiva é uma dermatose sem etiologia definida. Não há consenso ou medicação de primeira linha para o seu tratamento e os tratamentos utilizados são pouco eficazes. OBJETIVO: Avaliar a eficácia terapêutica da combinação tópica de peróxido de benzoíla 5% e clindamicina 1% associada à exposição solar para o tratamento da hipomelanose macular progressiva. MATERIAIS E MÉTODOS: Trata-se de um estudo randomizado, duplo-cego, placebo-controlado, no qual os pacientes foram divididos em dois grupos: o Grupo A utilizou a combinação tópica de peróxido de benzoíla 5% e clindamicina 1% e o Grupo B usou um creme gel como placebo. Os pacientes foram orientados à exposição solar diária, avaliados e fotografados sistematicamente. Os dados coletados foram inseridos e analisados pelo software Epi Info. Definiu-se a significância estatística por valor de pBACKGROUND: Progressive macular hypomelanosis is a dermatosis without definite etiology. There is no consensus or first-line therapy in the treatment of progressive macular hypomelanosis, and the treatment options used are very little effective. OBJECTIVE: To evaluate the therapeutic efficacy of the topical combination of benzoyl peroxide 5% and clindamycin 1% associated with sun exposure for the treatment of progressive macular hypomelanosis. MATERIALS AND METHODS: This is a randomized, double-blind, placebo-controlled study in which patients were divided into two groups. Group A used the topical combination of benzoyl peroxide 5% and clindamycin 1% and Group B used gel cream as a placebo. Patients were advised to expose themselves to the sun on a daily basis and were systematically evaluated and photographed. The collected data were entered and analyzed using Epi Info. A p value < 0.05 was considered statistically significant. RESULTS: Out of the 23 patients included in the study, 13 were in group A and 10 in group B. Eleven patients (85% in

  1. Estudo clínico, prospectivo, aberto, randomizado e comparativo para avaliar a segurança e a eficácia da luz azul versus peróxido de benzoíla 5% no tratamento da acne inflamatória graus II e III A prospective, randomized, open and comparative study to evaluate the safety and efficacy of blue light treatment versus a topical benzoyl peroxide 5% formulation in patients with acne grade II and III

    Directory of Open Access Journals (Sweden)

    Lúcia H. F. de Arruda

    2009-10-01

    Full Text Available FUNDAMENTOS: Muitos pacientes relatam melhora da acne com a exposição à luz solar, e vários estudos demonstram que a luz azul é efetiva no tratamento da acne. OBJETIVOS: Verificar a segurança e a eficácia da luz azul (espectro eletromagnético de 407 a 420 nm no tratamento da acne inflamatória graus II e III, comparada à terapêutica tópica com peróxido de benzoíla a 5%. MÉTODOS: O estudo avaliou 60 pacientes em cinco visitas: uma de seleção, uma com 7, 14 e 28 dias de tratamento e uma última de seguimento, 14 dias após o término do tratamento. Trinta foram randomizados para luz azul (oito sessões, duas vezes por semana, e outros 30, para peróxido de benzoíla a 5%, duas vezes ao dia, diariamente. A avaliação foi por meio da contagem das lesões e fotografias. RESULTADOS: A redução no número médio de lesões foi semelhante com os dois tratamentos, independente do tipo de lesão (p 0,05, porém o tratamento com a luz azul apresentou menos efeitos colaterais. CONCLUSÕES: A luz azul foi um tratamento tão eficaz quanto o peróxido de benzoíla a 5% para o tratamento da acne graus II e III, mas com menos efeitos adversos.BACKGROUND: Many acne patients improve after exposure to sunlight and there are many reports about the efficacy of blue light phototherapy on acne lesions. OBJECTIVES - The purpose of this study was to evaluate efficacy and safety of blue light treatment versus topical benzoyl peroxide 5% formulation in patients with acne grades II and III. METHODS - Sixty volunteers with facial acne were included and evaluated in 5 visits: the first one for screening, another 3 held on days 7, 14 and 28 of treatment, and the last one after 14 days of the end of treatment. Thirty of them were irradiated with Blue Light (8 times, twice a week and the other thirty were treated with topical Benzoyl Peroxide 5% formulation, auto-applied twice a day, every day. We assessed the severity of acne by counting the lesions and

  2. 1-苯甲酰基-3-(4,6-二甲氧基嘧啶-2-氨基)硫脲的合成、晶体结构及生物活性%Synthesis and Crystal Structure of 1-benzoyl-3-(4,6-dimethoxylpyrimidin-2-yl)thiourea

    Institute of Scientific and Technical Information of China (English)

    傅丁薇; 宋纪蓉; 任莹辉; 吕兴强; 胡怀明

    2007-01-01

      1-Benzoyl-3-(4,6-dimethoxylpyrimidin-2-yl)thiourea was synthesized with 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and benzoyl chloride in ethyl acetate. Its structure was characterized by X-ray diffraction analysis, which shows four molecules in each structural unit. The crystal belongs to triclinic, space group P⎯1 with a=0.9040(2)nm, b=1.8285(4)nm, c=1.8931(5) nm,α=70.217(4) º,β=80.583(4) º,γ=84.110(4)º, V=2901.3(12)Ǻ3, Dc=1.458 g/cm3,μ(MoKα)=0.242 mm-1, F(000)=1328, Z=8, R=0.0637, wR=0.1698 for 2095 observed reflections [FO>4sig(FO)]. The existence of the staggered intermolecular N—H⋅⋅⋅S (DA) and complementary C—H⋅⋅⋅O (DA) hydrogen bonds between the adjacent molecules in the same layer, together with the weak π⋅⋅⋅π stacking interactions between the near two layers, leads to the formation of multi-dimensional supramolecular networks. This type of compound has nice effect on growth regulation of wheat.%  以2-氨基-4,6-二甲氧基嘧啶、硫氰酸钾和苯甲酰氯为原料,在乙酸乙酯中合成了1-苯甲酰基-3-(4,6-二甲氧基嘧啶-2-氨基)硫脲,并用X射线单晶衍射法测定其晶体结构.结果表明每个结构单元中有4个分子,该化合物属于三斜系, P⎯1空间群,a=0.9040(2)nm, b=1.8285(4)nm, c=1.8931(5) nm,α=70.217(4)º,β=80.583(4)º,γ=84.110(4)º,V=2901.3(12)Ǻ3,Dc=1.458 g/cm3,μ=0.242 mm-1, F(000)=1328, Z=8,R=0.0637,由2095个可观测衍射点[FO>4sig(FO)]得到的wR=0.1698.同层中相邻分子间的分子间氢键N—H⋅⋅⋅S (DA)和C—H⋅⋅⋅O (DA)的交叉作用以及层与层之间弱的π⋅⋅⋅π堆积作用使得化合物形成网状超分子结构.该结构的化合物具有良好的生物活性.

  3. 4 '-acetyl benzo-15-crown-5 2-naphthyloxyacetyl hydrazone

    Institute of Scientific and Technical Information of China (English)

    ZHOU Yan-qing; WEI Tai-bao; ZHANG You-ming; ZONG Guo-qiang

    2004-01-01

    Aryloxyacetic acid and its derivatives often possess many important biological activities.Some of them are used as herbicides and plant-growth regulators. In continuation of our previous work on synthesis and biological activities1,2,3, we decided to design series of compounds containing the aryloxyacetyl group and crown ether to study the variation of bioactivities and the effect of the substituents on the ability of the crown ether to bind metal ions4,5. Recently, we determined related crystal structures6,7,8 , in order to study both bioactivities and coordination behaviour. In view of these encouraging results, the structure of the title compound (Figure 1), was obtained and is reported here.Figure 1 The molecule configuration and atom-numbering schem for the title compound,showing ellipsoids at the 50% probability level.Crystals of the ritle compound, C28H32N2O7, is monoclinic, space group P2(1)/c, a = 8.808(3), b =24.579(7), c =11.984(4), α = 90.00, β = 97.248(6), γ = 90.00, Z = 4, Dx= 1. 313 Mg m-3 ,Mo K α, λ =0.71073 , = 9.5mm-1 , F(000) = 1080, T =293(2) K, R = 0.0594, wR=0.1184 for 2575reflections [I>2 σ (Ⅰ) ] .The title compound adopts a syn-anti conformation, which enables N2-H...O6 intermolecule hydrogen bonds to be formed between centrosymmetrically related molecules. The resulting eight-membered rings join these molecules together as characteristic dimmers.

  4. Purification of benzoyl-mercaptoacetyltriglycine complemented with biological evaluations

    International Nuclear Information System (INIS)

    Purification was carried out by fractionated crystallization in metanol: water (80:20), monitored by HPLC. Many precipitations are obtained and used to prepare test small batchs marked with Tc-99m, and radiochemical controls and biological evaluations are performed. Results obtained as follows: the chemical purity of Bz-MAG3 is increased in 70% to 98.12% of the active component, with a performance of about 25%; radiochemical purity of the pure precipitations is higher than 98% and the percentage of injection dose in kidneys is increased from 8% to 20% at 5 minutes of the post-injection in healthy mice. The percentage of renal average excretion at 60 minutes is higher than 90%, percentage that will guarantee a good quality of renal radioisotope scanning

  5. Ethyl N-(2-benzoyl-3-oxo-3-phenylpropanoylcarbamate

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2013-02-01

    Full Text Available In the title compound, C19H17NO5, the dihedral angle between the phenyl groups is 79.55 (15°. The terminal ethoxy group is disordered over two orientations in a 0.873 (6:0.127 (6 ratio. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds into [001] chains which incorporate R12(6 loops. A very weak C—H...π contact also occurs.

  6. Benzoyl peroxide-induced damage to DNA and its components

    DEFF Research Database (Denmark)

    Hazlewood, C; Davies, Michael Jonathan

    1996-01-01

    radical generation, though there is controversy as to which radicals are responsible for this damage; previous workers have variously implicated benzoyloxyl (PhCO2,) phenyl (Ph.), and hydroxyl radicals (HO.) as the initiating agent. In the present study a detailed examination of the radicals generated on......, sugars, nucleosides, nucleotides, RNA, and DNA have been examined and the intermediate species have been identified in many cases. Comparison of these data with those obtained with Ph. alone has allowed the reactions of PhCO2. and Ph. to be distinguished. Evidence has been obtained which is consistent...... with both the addition of these radicals to the C5-C6 double bond of the pyrimidines to give adduct species, and hydrogen abstraction from the sugar rings. The former process is the major reaction for nucleosides and nucleotides. Studies with RNA and DNA also provide strong evidence for the formation...

  7. 3,9-Di-1-naphthyl-2,4,8,10-tetraoxaspiro[5.5]undecane

    Directory of Open Access Journals (Sweden)

    Xiuqin Zhang

    2010-05-01

    Full Text Available In the title compound, C27H24O4, the 1,3-dioxane rings have chair conformations. The molecule has non-crystallographic twofold rotation symmetry. The dihedral angle between the naphthalene ring systems is 17.96(4° In the crystal structure, weak intermolecular C—H...π interactions contribute to the crystal packing.

  8. ADSORPTION OF LATERALLY INTERACTING 1-NAPHTHOL/1-NAPHTHYL AMINE MIXTURES ON NONPOLAR SURFACES FROM AQUEOUS SOLUTIONS

    Institute of Scientific and Technical Information of China (English)

    Wei-ming Zhang; Jin-long Chen; Qun Chen; Ming-yang He; Bing-cai Pan; Quan-xing Zhang

    2006-01-01

    The binary adsorption behavior of 1-naphthol/1-naphthylamine mixtures in water on nonpolar adsorbent Amberlite XAD4 was investigated at 293 K, 303 K and 313 K, respectively. The experimental uptakes of 1-naphthol and 1-naphthylamine in all binary-component systems of different molar ratios were obviously higher than the corresponding uptakes predicted by the extended Langmuir model, assuming no interaction between the adsorbed molecules of the two components. This phenomenon was attributed to the cooperative adsorption effect arising from the hydrogen bonding interaction between 1-naphthol and 1-naphthylamine molecules. A modified extended Langmuir model was proposed to describe the binary adsorption behavior by means of introducing a fitting parameter related with the cooperative adsorption effect of the adsorbates.

  9. Disubstituted naphthyl β-D-xylopyranosides: Synthesis, GAG priming, and histone acetyltransferase (HAT) inhibition.

    Science.gov (United States)

    Thorsheim, Karin; Persson, Andrea; Siegbahn, Anna; Tykesson, Emil; Westergren-Thorsson, Gunilla; Mani, Katrin; Ellervik, Ulf

    2016-04-01

    Xylosides are a group of compounds that can induce glycosaminoglycan (GAG) chain synthesis independently of a proteoglycan core protein. We have previously shown that the xyloside 2-(6-hydroxynaphthyl)β-D-xylopyranoside has a tumor-selective growth inhibitory effect both in vitro and in vivo, and that the effect in vitro was correlated to a reduction in histone H3 acetylation. In addition, GAG chains have previously been reported to inhibit histone acetyltransferases (HAT). To investigate if xylosides, or the corresponding xyloside-primed GAG chains, can be used as HAT inhibitors, we have synthesized a series of naphthoxylosides carrying structural motifs similar to the aromatic moieties of the known HAT inhibitors garcinol and curcumin, and studied their biological activities. Here, we show that the disubstituted naphthoxylosides induced GAG chain synthesis, and that the ones with at least one free phenolic group exhibited moderate HAT inhibition in vitro, without affecting histone H3 acetylation in cell culture. The xyloside-primed GAG chains, on the other hand, had no effect on HAT activity, possibly explaining why the effect of the xylosides on histone H3 acetylation was absent in cell culture as the xylosides were recruited for GAG chain synthesis. Further investigations are required to find xylosides that are effective HAT inhibitors or xylosides producing GAG chains with HAT inhibitory effects. PMID:27023911

  10. Synthesis and Antimicrobial Activities of Some Novel Quinoxalinone Derivatives

    Directory of Open Access Journals (Sweden)

    Y. A. Ammar

    2000-06-01

    Full Text Available Condensation of 4-benzoyl-1,2-phenylenediamine with sodium pyruvate in acetic acid furnished two products which were identified as 6-benzoyl and 7-benzoyl-3-methyl-2(1Hquinoxalinones (1a,b. Fusion of 1a with aromatic aldehydes furnished the styryl derivatives 2a-c. Alkylation of 1a,b with dimethyl sulphate or ethyl chloroacetate produced the N-alkyl derivatives 3a,b and 4a,b. Hydrazinolysis of the ester derivative 4a with hydrazine hydrate afforded the hydrazide derivative 5 which underwent condensation with aldehydes to give the corresponding hydrazone derivatives 6a,b. In addition, chlorination of 1a with thionyl chloride afforded the 2-chloro derivative 7 which was subjected to reaction with sodium azide and n-butylamine to yield the corresponding tetrazolo (8 and n-butylamino (9 derivatives, respectively. The structures of the compounds prepared were confirmed by analytical and spectral data. Also, some of the synthesized compounds were screened for antimicrobial activity.

  11. SH groups in the alpha-naphthyl acetate esterase in the thyroid of the guinea-pig. A histochemical study

    DEFF Research Database (Denmark)

    Kirkeby, S

    1976-01-01

    cysteine was added to the incubation media in equivalent concentrations to the SH blocker. There were great differences among the sulfhydryl reagents used in their ability to bring about enzyme inhibition. The alkylating agents NEM (N-ethylmaleimide) and iodoacetamide had no or little effect while PCMB...

  12. N-(3-Bromo-1,4-dioxo-1,4-dihydro-2-naphthyl-2-chloro-N-(2-chlorobenzoylbenzamide

    Directory of Open Access Journals (Sweden)

    Emmanuel S. Akinboye

    2009-01-01

    Full Text Available The title compound, C24H12BrCl2NO4, was synthesized from 2-amino-3-bromo-1,4-naphthoquinone and 2-chlorobenzoyl chloride. The crystal structure shows that each of the chlorophenyl rings is inclined at about 60° to the naphthoquinone ring system. The two chlorophenyl rings adopt a conformation that ensures that chlorine substituents are anti so as to reduce electronic repulsion. An examination of the packing shows close O...Br and Cl...Cl contacts of 2.947 (2 and 3.346 (1 Å, respectively. In addition, the molecules are linked by weak intermolecular C—H...O and C—H...Cl interactions.

  13. Cytotoxicity, anti-angiogenic, apoptotic effects and transcript profiling of a naturally occurring naphthyl butenone, guieranone A

    Directory of Open Access Journals (Sweden)

    Kuete Victor

    2012-06-01

    Full Text Available Abstract Background Malignant diseases are responsible of approximately 13% of all deaths each year in the world. Natural products represent a valuable source for the development of novel anticancer drugs. The present study was aimed at evaluating the cytotoxicity of a naphtyl butanone isolated from the leaves of Guiera senegalensis, guieranone A (GA. Results The results indicated that GA was active on 91.67% of the 12 tested cancer cell lines, the IC50 values below 4 μg/ml being recorded on 83.33% of them. In addition, the IC50 values obtained on human lymphoblastic leukemia CCRF-CEM (0.73 μg/ml and its resistant subline CEM/ADR5000 (1.01 μg/ml and on lung adenocarcinoma A549 (0.72 μg/ml cell lines were closer or lower than that of doxorubicin. Interestingly, low cytotoxicity to normal hepatocyte, AML12 cell line was observed. GA showed anti-angiogenic activity with up to 51.9% inhibition of the growth of blood capillaries on the chorioallantoic membrane of quail embryo. Its also induced apotosis and cell cycle arrest. Ingenuity Pathway Analysis identified several pathways in CCRF-CEM cells and functional group of genes regulated upon GA treatment (P , the Cell Cycle: G2/M DNA Damage Checkpoint Regulation and ATM Signaling pathways being amongst the four most involved functional groups. Conclusion The overall results of this work provide evidence of the cytotoxic potential of GA and supportive data for its possible use in cancer chemotherapy.

  14. Synthesis, Structure and Thermochromic Properties of a Copper(Ⅱ) Complex Based on Naphthyl Carboxylate and Benzimidazolyl Ligands

    Institute of Scientific and Technical Information of China (English)

    YIN Fu-Jun; ZHAO Hong; XU Xing-You; YANG Xu-Jie

    2013-01-01

    One novel copper(Ⅱ) complex,[Cu(NAA)2(bim)2]·H2O (1,HNAA =a-naphthylacetic acid,bim =benzimidazole) has been synthesized and characterized by X-ray single-crystal diffraction analysis,elemental analysis,and IR spectrum.It crystallizes in monoclinic,space group C2/c with a =1.15969(12),b =1.9757(2),c =1.45763(16) nm,β =104.712(2)°,V=3.2298(6) nm3,Z =4,C38H32N4OsCu,Mr =688.22,Dc =1.418 g/cm-3,μ =0.729 mm-1,S =1.039,F(000) =1428,the final R =0.0380 and wR =0.0912 for 2849 unique reflections.In 1,two carboxylate and two benzimidazole ligands coordinate to the central Cu(Ⅱ) atom by a bidentate chelate mode.Interesting,reversible thermochromic properties of 1 can be observed and investigated by thermal analysis method.

  15. Part 1: Notch-sparing γ-secretase inhibitors: The identification of novel naphthyl and benzofuranyl amide analogs.

    Science.gov (United States)

    Lu, Dai; Wei, Han-Xun; Zhang, Jing; Gu, Yongli; Osenkowski, Pamela; Ye, Wenjuan; Selkoe, Dennis J; Wolfe, Michael S; Augelli-Szafran, Corinne E

    2016-05-01

    γ-Secretase is one of two proteases directly involved in the production of the amyloid β-peptide (Aβ), which is pathogenic in Alzheimer's disease. Inhibition of γ-secretase to suppress the production of Aβ should not block processing of one of its alternative substrates, Notch1 receptors, as interference with Notch1 signaling leads to severe toxic effects. In the course of our studies to identify γ-secretase inhibitors with selectivity for APP over Notch, 1 [3-(benzyl(isopropyl)amino)-1-(naphthalen-2-yl)propan-1-one] was found to inhibit γ-secretase-mediated Aβ production without interfering with γ-secretase-mediated Notch processing in purified enzyme assays. As 1 is chemically unstable, efforts to increase the stability of this compound led to the identification of 2 [naphthalene-2-carboxylic acid benzyl-isopropyl-amide] which showed similar biological activity to compound 1. Synthesis and evaluation of a series of amide analogs resulted in benzofuranyl amide analogs that showed promising Notch-sparing γ-secretase inhibitory effects. This class of compounds may serve as a novel lead series for further study in the development of γ-secretase inhibitors. PMID:27013392

  16. Synthesis, Structure Optimization and Antifungal Screening of Novel Tetrazole Ring Bearing Acyl-Hydrazones

    Directory of Open Access Journals (Sweden)

    Manzoor A. Malik

    2012-08-01

    Full Text Available Azoles are generally fungistatic, and resistance to fluconazole is emerging in several fungal pathogens. In an attempt to find novel azole antifungal agents with improved activity, a series of tetrazole ring bearing acylhydrazone derivatives were synthesized and screened for their in vitro antifungal activity. The mechanism of their antifungal activity was assessed by studying their effect on the plasma membrane using flow cytometry and determination of the levels of ergosterol, a fungal-specific sterol. Propidium iodide rapidly penetrated a majority of yeast cells when they were treated with the synthesized compounds at concentrations just above MIC, implying that fungicidal activity resulted from extensive lesions of the plasma membrane. Target compounds also caused a considerable reduction in the amount of ergosterol. The results also showed that the presence and position of different substituents on the phenyl ring of the acylhydrazone pendant seem to play a role on the antifungal activity as well as in deciding the fungistatic and fungicidal nature of the compounds.

  17. Derivative spectrophotometric determination of Ruthenium (III) using Diacetyl Monoxime Isonicotinoyl Hydrazone (DMIH)

    International Nuclear Information System (INIS)

    Ruthenium (III) forms a purple coloured water soluble complex with Diacetyl Monoxime Isonicotinoylhydrazone(DMIH) reagent in acidic buffer pH 4.5 with λmax at 346 nm. The molar absorptivity and Sandell's sensitivity are 1.4 X 104 L.mol-1.cm-1 and 0.0048 μg/cm2 respectively. The Beer's law validity range is 0.505 to 6.06 μg/ml. Ruthenium(III) forms (M:L) 1:1 complex with DMIH. Stability constant of the complex is 2.694X106. The derivative spectrophotometric determination of Ru(III) was carried out by measuring peak height method. The developed derivative spectrophotometric method was employed for the determination of Ruthenium (III) in synthetic samples of alloy and river water samples. The effect of various diverse ions is also studied. (author)

  18. Synthesis molecular modeling and anticonvulsant activity of some hydrazone, semicarbazone, and thiosemicarbazone derivatives of benzylidene camphor

    OpenAIRE

    Agrawal, Saurabh

    2014-01-01

    Saurabh Agrawal,1 Jainendra Jain,2 Ankit Kumar,3 Pratibha Gupta,4 Vikas Garg5 1Meerut Institute of Engineering and Technology, Meerut, Uttar Pradesh, India; 2Ram–Eesh Institute of Vocational and Technical Education, Greater Noida, Uttar Pradesh, India; 3Kharvel Subharti College of Pharmacy, Swami Vivekanand Subharti University, Meerut, Uttar Pradesh, India; 4Atarra Degree College, Atarra, Banda, India; 5Manipal College of Pharmaceutical Sciences, Manipal University, Manipal, Karnata...

  19. Antibacterial and Enzyme Inhibition Study of Hydrazone Derivatives Bearing 1, 3, 4-Oxadiazole

    Directory of Open Access Journals (Sweden)

    S. Rasool

    2015-03-01

    Full Text Available The antibacterial and lipoxygenase enzyme inhibition activities of two series of compounds have been investigated in the presented work. The 4-methyl/hydroxy benzoic acids (1a & 1b were used as starting materials to prepare corresponding esters (2a & 2b, hydrazides (3a & 3b, 5-(4-methylphenyl/4-hydroxyphenyl-1,3,4-oxadiazol-2-thiols (4a & 4b, S-substituted esters (5a & 5b and acetohydrazides (6a & 6b. The acetohydrazones, 8a-i & 9a-i, were synthesized by stirring 6a & 6b with mono(disubstituted phenylcarboxaldehydes (7a-i in methanol. The data of IR, 1H-NMR and EIMS spectral techniques well confirmed the structural formulae of synthesized compounds. The molecules of 4-methyl series rendered the better results than those of 4-hydroxy series.

  20. The DFT investigations of the electron injection in hydrazone-based sensitizers

    KAUST Repository

    Al-Sehemi, Abdullah G.

    2012-03-01

    Quantum chemical calculations were carried out by using density functional theory and time-dependant density functional theory at B3LYP/6-31G(d) and TD-B3LYP/6-31G(d) level of theories. The absorption spectra have been computed with and without solvent. The calculated absorption spectra in ethanol, acetonitrile, and methanol are in good agreement with experimental evidences. The absorption spectra are red shifted compared to System1. On the basis of electron injection and electronic coupling constant, we have shed light on the nature of different sensitizers. The coplanarity between the benzene near anchoring group having LUMO and the bridge (N-N) is broken in System6 and System7 that would hamper the recombination process. The electron injection of System2-System10 is superior to System1. The highest electronic coupling constant has been observed for System6 that followed the System7 and System8. The light-harvesting efficiency of all the sensitizers enlarged in acetonitrile and ethanol. The long-range-corrected functional (LC-BLYP), Coulomb-attenuating method (CAM-B3LYP), and BH and HLYP functional underestimate the excitation energies while B3LYP is good to reproduce the experimental data. Moreover, we have investigated the effect of cyanoacetic acid as anchoring group on the electron injection. © 2012 Springer-Verlag.

  1. Crystal structure, complexation, spectroscopic characterization and antimicrobial evaluation of 3,4-dihydroxybenzylidene isonicotinyl-hydrazone

    Science.gov (United States)

    Jeragh, Bakir; Ali, Mayada S.; El-Asmy, Ahmed A.

    2015-06-01

    A single crystal of 3,4-dihydroxybenzylidene isonicotinylhydrazone, HBINH, has been grown and solved by X-ray crystallography. The VO2+, Zr4+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Hg2+ and Pd2+ complexes of HBINH have been prepared and spectroscopically characterized. The data confirmed the formulae [Co(HBINH)(H2O)Cl]Cl·H2O, [Pd(HBINH)Cl2], [Zn(HBINH)2Cl2], [Cd(HBINH)(H2O)2Cl2]·1½H2O, [(VO)2(HBINH-3H)(OH)(H2O)], [Ni2(HBINH)(H2O)6Cl2]Cl2, [Cu2(HBINH-3H)(H2O)2(OAc)]·3H2O, [Zr2(HBINH-3H)Cl4]Cl, [Hg2(HBINH)Cl4] and the dimer {[Cu(HBINH)Cl]Cl}2. Most of the complexes have intense colors and high melting points and some are electrolytes in DMSO solution. The ligand behaves as a neutral bidentate in the Co(II), Cu(II), Pd(II), Zn(II) and Cd(II) complexes; dibasic tetradentate in [Ni2(HBINH)(H2O)6Cl2]Cl2 and tribasic tetradentate in [Cu2(HBINH-3H)(OAc)]·5H2O, [(VO)2(HBINH-3H)(OH)(H2O)] and [Zr2(HBINH-3H)Cl4]Cl by the loss of 3H+ due to the deprotonation of the two hydroxyl groups and the enolization of the amide (Odbnd CNH) group. A tetrahedral geometry was proposed for the Co(II), Cu(II), Zn(II) and Hg(II) complexes; square-planar for the Pd(II) complex; square-pyramid for the VO2+ complex and octahedral for the Ni(II) and Cd(II) complexes. The complexes [Cd(HBINH)(H2O)2Cl2]·1½H2O, [(VO)2(HBINH-3H)(OH)(H2O)] and [Cu2(HBINH-3H)-(H2O)2(OAc)]·3H2O have activities against Bacillus sp. M3010, Candida albicans, Escherichia coli, Staphylococcus aureus and Slamonella sp. PA393.

  2. Cyclisation reactions of hydrazones XXXII. Synthesis of some pyrazolylhydrazones and study of their cyclisation

    Czech Academy of Sciences Publication Activity Database

    Cankař, P.; Maloň, Michal; Gucký, Tomáš; Slouka, J.

    2011-01-01

    Roč. 142, č. 11 (2011), s. 1149-1153. ISSN 0026-9247 R&D Projects: GA AV ČR KAN200380801 Keywords : heterocycles * isomers * pyrazolo[5,1-c][1,2,4]triazine * pyrazolo[5,1-c]pyrimido[4,5-e][1,2,4]triazine Subject RIV: CC - Organic Chemistry Impact factor: 1.532, year: 2011

  3. Construction of an Asymmetric Quaternary Carbon Center via Allylation of Hydrazones

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jin Bum; Satyender, Apuri; Jang, Doo Ok [Yonsei Univ., Wonju (Korea, Republic of)

    2013-11-15

    Asymmetric indium-mediated allylation of imine derivatives bearing a chiral auxiliary is a reliable strategy for the synthesis of chiral homoallylic amines. Various techniques for indium-mediated stereoselective allylation of imines bearing a chiral auxiliary have been reported. In 1997 Loh and co-workers reported indium-mediated allylation with imines derived from L-valine methyl ester. Since then, many forms of indium-mediated allylation bearing a chiral auxiliary have been reported, including imines derived from (S)-valinol, (R)-phenylglycinol, uracil, (R)-phenylglycinol methyl ester, N-tert-butanesufinamide, and (1R,2S)-1-amino-2-indanol. However, the synthesis of chiral auxiliaries often involves a laborious multi-step synthesis with expensive reagents. Therefore, the development of readily accessible chiral auxiliaries for asymmetric indium-mediated all-ylation is in high demand.

  4. Aroylhydrazone iron chelators: Tuning antioxidant and antiproliferative properties by hydrazide modifications.

    Science.gov (United States)

    Hrušková, Kateřina; Potůčková, Eliška; Hergeselová, Tereza; Liptáková, Lucie; Hašková, Pavlína; Mingas, Panagiotis; Kovaříková, Petra; Šimůnek, Tomáš; Vávrová, Kateřina

    2016-09-14

    Aroylhydrazones such as salicylaldehyde isonicotinoyl hydrazone (SIH) are tridentate iron chelators that may possess antioxidant and/or antineoplastic activities. Their main drawback, their low stability in plasma, has recently been partially overcome by exchanging the aldimine hydrogen for an unbranched alkyl group. In this study, ten analogs of methyl- and ethyl-substituted SIH derivatives with modified hydrazide scaffolds were synthesized to further explore their structure-activity relationships. Their iron-chelation efficiencies, anti- or pro-oxidant potentials, abilities to induce protection against model oxidative injury on the H9c2 cell line derived from rat embryonic cardiac tissue, cytotoxicities on the same H9c2 cells and antiproliferative activities on MCF-7 human breast adenocarcinoma and HL-60 human promyelotic leukemia cell lines were evaluated. Compounds derived from lipophilic naphthyl and biphenyl hydrazides displayed highly selective antiproliferative activities against both MCF-7 and HL-60 cell lines, and they showed markedly improved stabilities in plasma compared to SIH. Of particular interest is a hydrazone prepared from 2-hydroxypropiophenone and pyridazin-4-carbohydrazide that showed a considerable antiproliferative effect and protected cardiomyoblasts against oxidative stress with a five-fold higher selectivity compared to the parent compound SIH. Thus, this work highlighted new structure-activity relationships among antiproliferative and antioxidant aroylhydrazones and identified new lead compounds for further development. PMID:27187862

  5. Extraction behavior of Am(III) in benzoyl pyrazolone dissolved in pyrolidnium ionic liquid

    International Nuclear Information System (INIS)

    Extraction of Am(III) from nitric acid medium was carried out in a solution of benzoylpyrazolone (HPMBP) dissolved in 1-butyl-3-methylpyrrolidinium bis(trifluoro-methanesulfonyl)imide ((C4mpyr)(NTf2)) ionic liquid. The extraction behavior of Am(III) in ionic liquid phase was investigated as a function of pH of the aqueous phase. The extraction behavior in ionic liquid was compared with those observed in n-dodecane and the stripping of Am(III) from the loaded ionic liquid phase was carried out using concentrated nitric acid. (author)

  6. ADSORPTION CHARACTERISTICS OF CHLOROPHENOLS FROM AQUATIC SYSTEMS BY HYPERCROSSLINKED RESINS MODIFIED WITH BENZOYL GROUP

    Institute of Scientific and Technical Information of China (English)

    Jing-ping Wang; Zheng-hao Fei

    2006-01-01

    A hypercrosslinked polymeric adsorbent (ZH-03) for adsorbing and removing chlorophenolic compounds from their aqueous solutions was studied, including the static adsorption. The equilibrium adsorption data were fit to Freundlich adsorption isothermic models to evaluate the model parameters. Thermodynamic studies on the adsorption of chlorophenolic compounds on ZH-03 indicated that there were chemisorption transitions for 2,4,6-trichlorophenol and physical adsorption processes for 2-chlorophenol and 2,6-chlorophenol, and ZH-03 showed the homogeneous nature of the adsorbent surface.Column adsorption for chlorophenols wastewater shows the advantages of the ZH-03 adsorbent for adsorbing the following chlorophenolic compounds as 2-chlorophenol, 2,6-dichlorophenol and 2,4,6-trichlorophenol. Sodium hydroxide was used for desorpting chlorophenols from ZH-03 and showed excellent performance.

  7. Synthesis, Cytotoxic and Antimalarial Activities of Benzoyl Thiosemicarbazone Analogs of Isoquinoline and Related Compounds

    Directory of Open Access Journals (Sweden)

    Somsak Ruchirawat

    2010-02-01

    Full Text Available Thiosemicarbazone analogs of papaveraldine and related compounds 1–6 were synthesized and evaluated for cytotoxic and antimalarial activities. The cytotoxic activity was tested against HuCCA-1, HepG2, A549 and MOLT-3 human cancer cell lines. Thiosemicarbazones 1–5 displayed cytotoxicity toward all the tested cell lines, while compounds 2–5 selectively showed potent activity against the MOLT-3 cell lines. Significantly, N(4-phenyl-2-benzoylpyridine thiosemicarbazone 4 exhibited the most potent activity against HuCCA-1, HepG2, A549 and MOLT-3 cell lines with IC50 values of 0.03, 4.75, 0.04 and 0.004 µg/mL, respectively. In addition, 2-benzoylpyridine thio-semicarbazones 3 and 4 showed antimalarial activity against Plasmodium falciparum with IC50 of 10-7 to < 10-6 M. The study demonstrates the quite promising activity of analog 4 as a lead molecule for further development.

  8. (±)-trans-3-Benzoyl-bicyclo-[2.2.2]octane-2-carboxylic acid.

    Science.gov (United States)

    Lalancette, Roger A; Thompson, Hugh W; Brunskill, Andrew P J

    2008-01-01

    The title keto acid, C(16)H(18)O(3), displays significant twisting of all three ethyl-ene bridges in its bicyclo-[2.2.2]octane structure owing to steric inter-actions; the bridgehead-to-bridgehead torsion angles are 13.14 (12), 13.14 (13) and 9.37 (13)°. The compound crystallizes as centrosymmetric carboxyl dimers [O⋯O = 2.6513 (12) Å and O-H⋯O = 178°], which have two orientations within the cell and contain no significant carboxyl disorder. PMID:21201657

  9. (2E-N′-Benzoyl-3-(4-nitrophenylprop-2-enohydrazide

    Directory of Open Access Journals (Sweden)

    Samir A. Carvalho

    2010-01-01

    Full Text Available In the title compound, C16H13N3O4, the dihedral angle between the terminal benzene rings is 14.02 (7°. The carbonyl groups are anti with respect to each other, which facilitates their participation in the formation of supramolecular chains. Each side of the –C(=ON(HN(HC(=O– residue associates with a centrosymmetrically related molecule, resulting in the formation of essentially flat ten-membered {...O=CNN(H}2 synthons. The resultant chains are further consolidated in the crystal structure via C—H...O contacts.

  10. Crystal structure of N-(3-benzoyl-4,5,6,7-tetrahydro-1-benzothiophen-2-ylbenzamide

    Directory of Open Access Journals (Sweden)

    Manpreet Kaur

    2014-09-01

    Full Text Available In the title compound, C22H19NO2S, the cyclohexene ring adopts a half-chair conformation. The dihedral angles between the plane of the thiophene ring and those of its amide- and carbonyl-bonded benzene rings are 7.1 (1 and 59.0 (2°, respectively. An intramolecular N—H...O hydrogen bond generates an S(6 ring. In the crystal, very weak aromatic π–π stacking interactions [centroid–centroid separation = 3.9009 (10 Å] are observed.

  11. Photocarcinogenesis and toxicity of benzoyl peroxide in hairless mice after simulated solar radiation

    DEFF Research Database (Denmark)

    Lerche, Catharina M; Philipsen, Peter A; Poulsen, Thomas;

    2010-01-01

    with UV radiation. BPO can promote skin tumorigenesis in a mouse skin chemical carcinogenesis model. As acne vulgaris is frequently localized on sun-exposed areas, we investigated whether BPO or BPO-clin accelerates photocarcinogenesis in combination with simulated solar radiation (SSR) in 12 groups of...

  12. Spectrophotometric determination of cobalt in aqueous solutions using di-2-pyridyl ketone derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Al-Nuri, M.A.; Abu-Eid, Maher; Zatar, N.A.; Khalaf, Shukri; Hannoun, Mohammed (An-Najah N. University, Nablus, West Bank (Israel). Chemistry Department); Khamis, Mustafa (College of Science and Technology, Abu-Dis, West Bank (Israel))

    1992-04-05

    A method for the spectrophotometric determination of cobalt(II) is presented, with a comparison of the binary complexes formed by cobalt (II) with di-2-pyridyl ketone nicotinoylhydrazone (DPKNH), di-2-pyridyl ketone 2-thiophenoylhydrazone (DPKTH) and di-2-pyridyl ketone benzoyl-hydrazone (DPKBH) in 50% (v/v) ethanolic solution. Cobalt(II) forms 1:2 complexes with the three reagents. Maximum absorbance is at 372 nm for Co(II)-DPKNH, at 389 nm for Co(II)-DPKTH and at 370 nm for Co(II)-DPKBH. Ranges of linearity, effects of pH and excess reagent, sensitivity, stability of the complexes and tolerance limits of ions are reported. It was concluded that the system with DPKTH is the best, followed by DPKNH and then DPKBH. The method was applied to the determination of cobalt in different alloys. (author). 17 refs.; 1 fig.; 3 tabs.

  13. Spectrophotometric determination of cobalt in aqueous solutions using di-2-pyridyl ketone derivatives

    International Nuclear Information System (INIS)

    A method for the spectrophotometric determination of cobalt(II) is presented, with a comparison of the binary complexes formed by cobalt (II) with di-2-pyridyl ketone nicotinoylhydrazone (DPKNH), di-2-pyridyl ketone 2-thiophenoylhydrazone (DPKTH) and di-2-pyridyl ketone benzoyl-hydrazone (DPKBH) in 50% (v/v) ethanolic solution. Cobalt(II) forms 1:2 complexes with the three reagents. Maximum absorbance is at 372 nm for Co(II)-DPKNH, at 389 nm for Co(II)-DPKTH and at 370 nm for Co(II)-DPKBH. Ranges of linearity, effects of pH and excess reagent, sensitivity, stability of the complexes and tolerance limits of ions are reported. It was concluded that the system with DPKTH is the best, followed by DPKNH and then DPKBH. The method was applied to the determination of cobalt in different alloys. (author). 17 refs.; 1 fig.; 3 tabs

  14. Glucopyranosylidene-spiro-iminothiazolidinone, a new bicyclic ring system: synthesis, derivatization, and evaluation for inhibition of glycogen phosphorylase by enzyme kinetic and crystallographic methods.

    Science.gov (United States)

    Czifrák, Katalin; Páhi, András; Deák, Szabina; Kiss-Szikszai, Attila; Kövér, Katalin E; Docsa, Tibor; Gergely, Pál; Alexacou, Kyra-Melinda; Papakonstantinou, Maria; Leonidas, Demetres D; Zographos, Spyros E; Chrysina, Evangelia D; Somsák, László

    2014-08-01

    The reaction of thiourea with O-perbenzoylated C-(1-bromo-1-deoxy-β-D-glucopyranosyl)formamide gave the new anomeric spirocycle 1R-1,5-anhydro-D-glucitol-spiro-[1,5]-2-imino-1,3-thiazolidin-4-one. Acylation and sulfonylation with the corresponding acyl chlorides (RCOCl or RSO₂Cl where R=tBu, Ph, 4-Me-C₆H₄, 1- and 2-naphthyl) produced the corresponding 2-acylimino- and 2-sulfonylimino-thiazolidinones, respectively. Alkylation by MeI, allyl-bromide and BnBr produced mixtures of the respective N-alkylimino- and N,N'-dialkyl-imino-thiazolidinones, while reactions with 1,2-dibromoethane and 1,3-dibromopropane furnished spirocyclic 5,6-dihydro-imidazo[2,1-b]thiazolidin-3-one and 6,7-dihydro-5H-thiazolidino[3,2-a]pyrimidin-3-one, respectively. Removal of the O-benzoyl protecting groups by the Zemplén protocol led to test compounds most of which proved micromolar inhibitors of rabbit muscle glycogen phosphorylase b (RMGPb). Best inhibitors were the 2-benzoylimino- (Ki=9μM) and the 2-naphthoylimino-thiazolidinones (Ki=10 μM). Crystallographic studies of the unsubstituted spiro-thiazolidinone and the above most efficient inhibitors in complex with RMGPb confirmed the preference and inhibitory effect that aromatic (and especially 2-naphthyl) derivatives show for the catalytic site promoting the inactive conformation of the enzyme. PMID:25009003

  15. Photocatalytic generation of N-centered hydrazonyl radicals: a strategy for hydroamination of β,γ-unsaturated hydrazones.

    Science.gov (United States)

    Hu, Xiao-Qiang; Chen, Jia-Rong; Wei, Qiang; Liu, Feng-Lei; Deng, Qiao-Hui; Beauchemin, André M; Xiao, Wen-Jing

    2014-11-01

    A visible-light photocatalytic generation of N-centered hydrazonyl radicals has been accomplished for the first time. This approach allows efficient intramolecular addition of hydrazonyl radical to terminal alkenes, thus providing hydroamination and oxyamination products in good yields. Importantly, the protocol involves deprotonation of an N-H bond and photocatalytic oxidation to an N-centered radical, thus obviating the need to prepare photolabile amine precursors or the stoichiometric use of oxidizing reagents. PMID:25513705

  16. Synthesis and Crystal Structure of a New cis-Dioxovanadium (V) Complex with Pyruvic Acid Isonicotinyl Hydrazone (PAINH)

    Institute of Scientific and Technical Information of China (English)

    CHEN Rui-Jin; ZHOU Yin-Zhuang; HU Dai-Di; TU Shu-Jie; XIAO Ling-Mei

    2006-01-01

    A new cis-dioxovanadium (V) complex [VO2(C9H8N3O3)](C5H5N) involving a carboxyl group coordination employing a tridentate Schiff Base derived from pyruvic acid and isonicotinyl hydrazide is reported. This complex crystallizes in triclinic, space group P(1-) with a = 7.3522 (12), b = 7.8376(13), c = 14.898(2)(A), α= 84.010(2),β= 86.568(2), γ = 64.586(2)°, V = 771.1(2)(A)3, Z = 2, F(000) = 376, Mr = 368.22, Dc = 1.586 g/cm3, μ = 0.677 mm-1, R = 0.0421 and wR = 0.1253. The vanadium atom of the dioxovanadium (V) is five-coordinated to furnish a distorted trigonal bipyramid geometry.

  17. Crystal Violet Lactone Salicylaldehyde Hydrazone Zn(II) Complex: a Reversible Photochromic Material both in Solution and in Solid Matrix

    Science.gov (United States)

    Li, Kai; Li, Yuanyuan; Tao, Jing; Liu, Lu; Wang, Lili; Hou, Hongwei; Tong, Aijun

    2015-09-01

    Crystal violet lactone (CVL) is a classic halochromic dye which has been widely used as chromogenic reagent in thermochromic and piezochromic systems. In this work, a very first example of CVL-based reversible photochromic compound was developed, which showed distinct color change upon UV-visible light irradiation both in solution and in solid matrix. Moreover, metal complex of CVL salicylaldehyde hydrozone was facilely synthesized, exhibiting reversible photochromic properties with good fatigue resistance. It was served as promising solid material for photo-patterning.

  18. Crystal Violet Lactone Salicylaldehyde Hydrazone Zn(II) Complex: a Reversible Photochromic Material both in Solution and in Solid Matrix

    OpenAIRE

    Kai Li; Yuanyuan Li; Jing Tao; Lu Liu; Lili Wang; Hongwei Hou; Aijun Tong

    2015-01-01

    Crystal violet lactone (CVL) is a classic halochromic dye which has been widely used as chromogenic reagent in thermochromic and piezochromic systems. In this work, a very first example of CVL-based reversible photochromic compound was developed, which showed distinct color change upon UV-visible light irradiation both in solution and in solid matrix. Moreover, metal complex of CVL salicylaldehyde hydrozone was facilely synthesized, exhibiting reversible photochromic properties with good fati...

  19. Synthesis, magnetic and spectral studies of lanthanide(III) chloride complexes of hydrazones of isonicotinic acid hydrazide

    International Nuclear Information System (INIS)

    The synthesis, magnetic and spectral properties of trivalent lanthanide chlorides with N-isonicotinamidobenzalaldimine (INH-BENZ), N-isonicotinamidoanisalaldimine (INH-ANSL) and N-isonicotinamido-p-dimethylaminobenzalaldimine (INH-PDAB) are described. 13 refs., 2 tabs

  20. Molecular design of new hydrazone dyes for dye-sensitized solar cells: Synthesis, characterization and DFT study

    KAUST Repository

    Al-Sehemi, Abdullah G.

    2012-07-01

    Three new sensitizers 2-{4-[2-(4-Nitrobenzylidene)hydrazino)]phenyl} ethylene-1,1,2-tricarbonitrile (NBHPET), 2-{4-[2-p-Chlorobenzylidenehydrazino] phenyl}- ethylene-1,1,2-tri carbonitrile (CBHPET) and 2-{4-[2-p- Bromobenzylidenehydrazino] phenyl}ethylene-1,1,2-tricarbonitrile (BBHPET) have been synthesized. The dyes showed pronounced solvatochromic effects as the polarity of the solvents increased. The structures have been optimized at B3LYP/6-31G(d) level of theory. The torsion in E-isomer is smaller than Z-isomer and azo isomers. The highest occupied molecular orbitals are delocalized on whole molecule while lowest unoccupied molecular orbitals are distributed on the tricarbonitrile. The lowest unoccupied molecular orbital energies are above the conduction band of titanium dioxide, highest occupied molecular orbitals of the dyes are below the redox couple of new synthesized dyes and small energy gap revealed these dyes would be better sensitizers for dye-sensitized solar cells. © 2012 Elsevier B.V. All rights reserved.

  1. (E)-1-Phenyl­butan-2-one (2,4-dinitro­phen­yl)hydrazone

    OpenAIRE

    Lima, Carlos F. R. A. C.; Gomes, Ligia R.; Santos, Luís M. N. B. F.; Rodriguez-Borges, José E.; Low, John Nicolson

    2009-01-01

    In the title compound, C16H16N4O4, the dihedral angle between the aromatic rings is 79.04 (8)° and an intra­molecular N—H⋯O hydrogen bond occurs. In the crystal, weak C—H.·O and C—H..π inter­actions link the mol­ecules, forming sheets.

  2. Comparison of the efficacy and safety of topical clindamycin and 5% benzoyl peroxide with nadifloxacin cream and 5% benzoyl peroxide gel in the treatment of acne vulgaris and assessment of the effects of these treatments on quality of life

    OpenAIRE

    Aslıhan Kırkağaç; Zeynep Nurhan Saraçoğlu; Ayşe Esra Koku Aksu

    2015-01-01

    Background and Design: Acne vulgaris is a multifactorial chronic inflammatory disase of the pilosebaceous unit. Topical antibiotics and anti-inflammatory treatment are used for mild and moderate acne. Clindamycin is frequently used for acne treatment, altough nadifloxacin is a relatively new agent. There are few studies evaluating nadifloxacin efficacy. It's impact on quality of life has not been determined previously. In this study, it is aimed to compare the effect of these two agents, and ...

  3. Application of 8-amino-N-(2-hydroxybenzylidene)naphthyl amine as a neutral ionophore in the construction of a lanthanum ion-selective sensor

    Energy Technology Data Exchange (ETDEWEB)

    Ganjali, M.R. [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of)]. E-mail: ganjali@khayam.ut.ac.ir; Norouzi, P. [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Alizadeh, T. [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Adib, M. [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of)

    2006-08-25

    In this work, a novel La(III) membrane sensor based on 8-amino-N-(2-hydroxybenzylidene)naphthylamine (AIP) is presented. This electrode reveals good selectivity for La{sup 3+} over a wide variety of lanthanides metal ions. Theoretical calculations and conductance study of AIP to lanthanum and some other metal ions were carried out and confirmed selectivity toward La(III) ions. The electrode comprises 7% AIP, 30% PVC, 61% NPOE and 2% KTpClPB. The sensor displays a linear dynamic range between 1.0 x 10{sup -7} and 1.0 x 10{sup -1} M, with a nice Nernstian slope of 20.3 {+-} 0.3 mV per decade and a detection limit of 8.0 x 10{sup -8} M. The potentiometric response is independent of pH in the range of 4.0-9.0. The proposed sensor posses the advantage of short response time, and especially, very good selectivity towards a large number of cations, such as Sm(III), Ce(III, Pr(III), Yb(III) and Hg(II), low detection limit and wide linear dynamic range in comparison with former ones. The electrode can be used for at least seven weeks without any considerable divergence in the potentials. It was used as an indicator electrode in the potentiometric titration of La(III) ions with EDTA. The sensor was applied to the determination of La(III) ions concentration in binary mixtures. It was also applied for the determination of fluoride ions in mouth wash preparations.

  4. A turn-on fluorescent anion receptor based on N,N'-di-β-naphthyl-1,10-phenanthroline-2,9-diamide

    International Nuclear Information System (INIS)

    A simple turn-on fluorescent anion chemosensor with amide moiety as binding sites was designed, synthesized and characterized. Binding ability of the receptor 1 with anions was evaluated through the fluorescence titration in DMSO and the 1H NMR titration in DMSO-d6 and coordination of anions to 1 led to a visible enhancement in fluorescence intensity. The fluorescence enhancement could be explained on the basis of two signaling transduction mechanisms: (1) inhibition of a photoinduced electronic transfer (PET) mechanism and (2) anion-induced increase of the rigidity of the host molecules. In addition, the results of 1H NMR titrations suggested that a host-guest hydrogen-bonding complex with an association constant Kass=7379 mol-1 L was formed between 1 and F- and the mode of host-guest interactions was provided

  5. DESIGN AND SYNTHESIS OF 4-[2’-(5’- NITRO] IMIDAZOLYL BENZOYL (N-METHYL AMINO ACIDS AND PEPTIDES

    Directory of Open Access Journals (Sweden)

    PARAMITA DAS

    2010-06-01

    Full Text Available In the past two decades, a wide variety of bioactive peptides have been discovered. Condensation of heterocyclic moieties viz nicotinic acid, thiazole coumarin, quinolin, furan, imidazole etc. with amino acids and peptides resulted in compounds with potent biological activities. Many of the heterocyclic found to exhibit antifungal, antibacterial, cytotoxic, antineoplastic, insectisidal, antiinflammatory, anthelmintic, tyrosinase inhibitory and melanin production inhibitory activities. Metronidazole, serconidazole, flucanazole are well known marketed drugs. Introduction of D-amino acids and N-methylation of amino acids like tyrosine, valine, alanine etc enhanced antimicrobial activity. Hence an attempt is made towards the synthesis of 5-nitroimidazolyl-benzoic acid derivative of N-methylamino acids and peptide using solution phase technique of peptide synthesis. The method includes the introduction of tert-butyloxy carboxyl group (Boc to amino acids to protect the amino group forming Boc-amino acids .The protection of carboxyl group was done by converting the amino acids into corresponding methyl ester. The protected amino acids were coupled using diisopropylcarbodimide and triethylamine to get protected dipeptides. N-methylation was done by treating with methyl iodide and sodium hydride. The ester group was then removed by lithium hydroxide. The Boc(N-methyldipetide were coupled to amino acids or Boc(Nmethyl dipeptide were coupled to 4-[2-(5-nitroimidazoly]benzoic acids.

  6. Rapid determination and chemical change tracking of benzoyl peroxide in wheat flour by multi-step IR macro-fingerprinting

    Science.gov (United States)

    Guo, Xiao-Xi; Hu, Wei; Liu, Yuan; Sun, Su-Qin; Gu, Dong-Chen; He, Helen; Xu, Chang-Hua; Wang, Xi-Chang

    2016-02-01

    BPO is often added to wheat flour as flour improver, but its excessive use and edibility are receiving increasing concern. A multi-step IR macro-fingerprinting was employed to identify BPO in wheat flour and unveil its changes during storage. BPO contained in wheat flour (< 3.0 mg/kg) was difficult to be identified by infrared spectra with correlation coefficients between wheat flour and wheat flour samples contained BPO all close to 0.98. By applying second derivative spectroscopy, obvious differences among wheat flour and wheat flour contained BPO before and after storage in the range of 1500-1400 cm- 1 were disclosed. The peak of 1450 cm- 1 which belonged to BPO was blue shifted to 1453 cm- 1 (1455) which belonged to benzoic acid after one week of storage, indicating that BPO changed into benzoic acid after storage. Moreover, when using two-dimensional correlation infrared spectroscopy (2DCOS-IR) to track changes of BPO in wheat flour (0.05 mg/g) within one week, intensities of auto-peaks at 1781 cm- 1 and 669 cm- 1 which belonged to BPO and benzoic acid, respectively, were changing inversely, indicating that BPO was decomposed into benzoic acid. Moreover, another autopeak at 1767 cm- 1 which does not belong to benzoic acid was also rising simultaneously. By heating perturbation treatment of BPO in wheat flour based on 2DCOS-IR and spectral subtraction analysis, it was found that BPO in wheat flour not only decomposed into benzoic acid and benzoate, but also produced other deleterious substances, e.g., benzene. This study offers a promising method with minimum pretreatment and time-saving to identify BPO in wheat flour and its chemical products during storage in a holistic manner.

  7. (2R,3R-3-O-Benzoyl-N-benzyltartramideTartaric acid and its O-acyl derivatives. Part 13.

    Directory of Open Access Journals (Sweden)

    Izabela D. Madura

    2012-06-01

    Full Text Available The title compound, C18H17NO6 [systematic name: (2R,3R-4-benzylamino-2-benzoyloxy-3-hydroxy-4-oxobutanoic acid], is the first structurally characterized unsymmetrical monoamide–monoacyl tartaric acid derivative. The molecule shows a staggered conformation around the tartramide Csp3—Csp3 bond with trans-oriented carboxyl and amide groups. The molecular conformation is stabilized by an intramolecular N—H...O hydrogen bond. In the crystal, molecules are linked by O—H...O hydrogen bonds between the carboxyl and amide carbonyl groups, forming translational chains along [001]. Further O—H...O and N—H...O hydrogen bonds as well as weaker C—H...O and C—H...π intermolecular interactions extend the supramolecular assembly into a double-layer structure parallel to (100. There are no directional interactions between the double layers.

  8. High activity of iron containing metal-organic-framework in acylation of p-xylene with benzoyl chloride

    Czech Academy of Sciences Publication Activity Database

    Kurfiřtová, Lenka; Seo, Y.; K.; Hwang, Y. K.; Chang, J.; S.; Čejka, Jiří

    2012-01-01

    Roč. 179, č. 1 (2012), s. 85-90. ISSN 0920-5861 R&D Projects: GA ČR GA104/07/0383 Institutional research plan: CEZ:AV0Z40400503 Keywords : acylation * p-xylene * zeolites Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.980, year: 2012

  9. Rapid determination and chemical change tracking of benzoyl peroxide in wheat flour by multi-step IR macro-fingerprinting.

    Science.gov (United States)

    Guo, Xiao-Xi; Hu, Wei; Liu, Yuan; Sun, Su-Qin; Gu, Dong-Chen; He, Helen; Xu, Chang-Hua; Wang, Xi-Chang

    2016-02-01

    BPO is often added to wheat flour as flour improver, but its excessive use and edibility are receiving increasing concern. A multi-step IR macro-fingerprinting was employed to identify BPO in wheat flour and unveil its changes during storage. BPO contained in wheat flour (flour and wheat flour samples contained BPO all close to 0.98. By applying second derivative spectroscopy, obvious differences among wheat flour and wheat flour contained BPO before and after storage in the range of 1500-1400 cm(-1) were disclosed. The peak of 1450 cm(-1) which belonged to BPO was blue shifted to 1453 cm(-1) (1455) which belonged to benzoic acid after one week of storage, indicating that BPO changed into benzoic acid after storage. Moreover, when using two-dimensional correlation infrared spectroscopy (2DCOS-IR) to track changes of BPO in wheat flour (0.05 mg/g) within one week, intensities of auto-peaks at 1781 cm(-1) and 669 cm(-1) which belonged to BPO and benzoic acid, respectively, were changing inversely, indicating that BPO was decomposed into benzoic acid. Moreover, another autopeak at 1767 cm(-1) which does not belong to benzoic acid was also rising simultaneously. By heating perturbation treatment of BPO in wheat flour based on 2DCOS-IR and spectral subtraction analysis, it was found that BPO in wheat flour not only decomposed into benzoic acid and benzoate, but also produced other deleterious substances, e.g., benzene. This study offers a promising method with minimum pretreatment and time-saving to identify BPO in wheat flour and its chemical products during storage in a holistic manner. PMID:26519920

  10. Synthesis, Antioxidant Activity and Fluorescence Properties of Novel Europium Complexes with (E)-2- or 4-hydroxy-N'-[(2-hydroxynaphthalen-1-yl)methylene]benzohydrazide Schiff Base

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Lijun [Ningxia Univ., Yinchuan (China); Alam, Mohammad Sayed [Jagannath Univ., Dhaka (Bangladesh); Lee, Dongung [Dongguk Univ., Gyeongju (Korea, Republic of)

    2012-10-15

    Two novel Eu(III) complexes with notable properties have been successfully prepared with hydrazone Schiff base ligands, (E)-2-hydroxy-N'-[(2-hydroxynaphthalen-1-yl)methylene]benzohydrazide (3a) and (E)-4-hydroxy-N'-[(2-hydroxynaphthalen-1-yl)methylene]benzohydrazide (3b). DFT, FMO energy and Mulliken charge distribution studies of the ligands allowed us to hypothesize that their HC=N, >C=O and -OH (naphthyl) groups were involved in coordinating with the Eu{sup 3+} ion. The eight coordination sites of the Eu{sup 3+} ion were occupied by the three functional groups of the two ligands (3a or 3b) mentioned above and two water molecules. Similar UV, IR and fluorescence spectra indicated the presence of comparable coordination environments for the Eu{sup 3+} ion in both complexes. Both the ligands and their complexes exhibited moderate DPPH radical scavenging activity. Moreover, it was found that the Eu(III) complexes exhibited fluorescence properties.

  11. An ESR study of the gamma radiolysis of aromatic polyesters containing isomeric naphthalene links

    International Nuclear Information System (INIS)

    Six polyesters were synthesised from 4,4'-oxy-bis(benzoyl chloride) and 1,4-, 1,5-, 1,6-, 2,3-, 2,6-, and 2,7-naphthalenediol isomers. The structures of the polyesters were characterised by means of IR, inherent viscosities in tetrachloroethane (TCE), solutions at 303 K and thermal analysis. The glass transition temperatures were in the range of 425-494 K by DSC thermal analysis. All of the polyesters were irradiated in an AECL Gammacell 220 unit at a dose rate of approximately 6.7 kGy/h to doses in the range of 0-15 kGy at 77 and 300 K. ESR spectroscopy was used to examine the radicals formed during radiolysis and to measure their yields. The G-values for radical formation in the polyesters were found to be in the range 0.18-1.41 at 77 K and 0.19-0.78 at 300 K. At 77 K, up to 15% of the radicals formed on radiolysis were found to be photo-bleachable anion radicals. Annealing experiments were carried out in order to identify the neutral radicals, which were assigned to naphthyl- or phenyl- and phenoxyl-type radicals

  12. Association between periodontal disease and cardiovascular disease

    International Nuclear Information System (INIS)

    Studies have supported the notion that subjects with periodontitis and patients with multiple tooth extractions as a result of chronic advanced periodontal disease (PDD) have a greater risk of developing Cardiovascular disease (CVD) than those who had little or no periodontal infection. Periodontitis may predispose affected patients to CVD by elevating systemic C-reactive protein level and pro-inflammatory activity in atherosclerotic lesions and accelerate development of cardiovascular diseases, Oral health variables including loss of teeth, positive plaque Benzoyl-D-L-Arginine- Naphthyl Amide test (BANA) scores, and compliant of xerostomia may by considered as risk indicators for CVD. Exact mechanism which links PDD and CVD has not been firmly established. The link between PDD and CVD may be attributed to bacteria entering blood stream and attaching to the fatty plaque in coronary artery and contributing to clot formation which can lead to heart attack. Inflammation caused by PDD increases the plaque build up. The association between the two disease entities is cause for concern. However, dental and medical practitioners should be aware of these findings to move intelligently to interact with inquiring patients with periodontitis. They should be urged to maintain medical surveillance of their cardiovascular status, and work on controlling or reducing all known risk factors associated with CVD, including periodontal infection. (author)

  13. Copper(II) complexes with 4-hydroxyacetophenone-derived acylhydrazones: Synthesis, characterization, DNA binding and cleavage properties

    Science.gov (United States)

    Gup, Ramazan; Gökçe, Cansu; Aktürk, Selçuk

    2015-01-01

    Two new Cu(II) complexes of Schiff base-hydrazone ligands, hydroxy-N‧-[(1Z)-1-(4-hydroxyphenyl)ethylidene]benzohydrazide [H3L1] and ethyl 2-(4-(1-(2-(4-(2-ethoxy-2-oxoethoxy)benzoyl)hydrazono)ethyl)phenoxy)acetate (HL2) have been synthesized and then characterized by microcopy and spectral studies. X-ray powder diffraction illustrates that [Cu(L2)2] complex is crystalline in nature whereas [Cu(H2L1)2]·2H2O has an amorphous structure. Binding of the copper complexes with Calf thymus DNA (CT-DNA) has been investigated by UV-visible spectra, exhibiting non-covalent binding to CT-DNA. DNA cleavage experiments have been also investigated by agarose gel electrophoresis in the presence and absence of an oxidative agent (H2O2). The effect of complex concentration on the DNA cleavage reaction has been also studied. Both copper complexes show nuclease activity, which significantly depends on concentrations of the complexes, in the presence of H2O2 through oxidative mechanism whereas they slightly cleavage DNA in the absence an oxidative agent.

  14. Synthesis, anti-inflammatory, analgesic and anticonvulsant activities of some new 4,6-dimethoxy-5-(heterocyclesbenzofuran starting from naturally occurring visnagin

    Directory of Open Access Journals (Sweden)

    E.R. El-Sawy

    2014-12-01

    Full Text Available Novel 3-(4,6-dimethoxybenzofuran-5-yl-1-phenyl-1H-pyrazole-4-carboxaldehyde (3 and 3-chloro-3-(4,6-dimethoxybenzofuran-5-ylpropenal (4 were prepared via Vilsmeier–Haack reaction of 1-(4,6-dimethoxybenzofuran-5-ylethanone (1 and its hydrazone derivative 2. Reaction of compound 4 with some hydrazine derivatives, namely hydrazine hydrate, phenylhydrazine and benzylhydrazine hydrochloride led to the formation of pyrazole derivatives 5–8, respectively. On the other hand, reaction of compound 4 with thiourea, urea or guanidine gave the pyrimidine derivatives 9–11, respectively. Reaction of amino compound 11 with acetic anhydride, benzoyl chloride and benzenesulphonyl chloride yielded N-substituted pyrimidine derivatives 12–14, respectively. Reaction of diazonium salt of compound 11 with sodium azide afforded azidopyrimidine derivative 15, which upon reaction with ethyl acetoacetate gave 1,2,3-triazole derivative 16. Acid catalyzed reaction of 11 with p-nitrobenzaldehyde gave Schiff base 17, which cyclized upon reaction with thioglycolic acid or chloroacetyl chloride to give thiazolidin-4-one 18 and azetidin-2-one 19, respectively. The newly synthesized compounds were tested for their anti-inflammatory, analgesic and anticonvulsant activities. Depending on the obtained results, the newly synthesized compounds possess significant anti-inflammatory, analgesic and anticonvulsant activities.

  15. Development of a strategy for the asymmetric synthesis of polycyclic polyprenylated acylphloroglucinols via N-amino cyclic carbamate hydrazones: application to the total synthesis of (+)-clusianone.

    Science.gov (United States)

    Garnsey, Michelle R; Lim, Daniel; Yost, Julianne M; Coltart, Don M

    2010-11-19

    A broadly applicable asymmetric synthetic strategy utilizing N-amino cyclic carbamate alkylation that provides access to the various stereochemical permutations of a common structural motif found in many polycyclic polyprenylated acylphloroglucinols is described. The utility of this methodology is demonstrated through the first asymmetric total synthesis of the antiviral agent (+)-clusianone. PMID:20977254

  16. Chromium(III), manganese(III), iron(III), oxovanadium(II), zirconium(IV) and dioxouranium(II) complexes of hydrazone of isonicotinic acid hydrazide

    International Nuclear Information System (INIS)

    Coordination complexes of Cr(III), Mn(III), Fe(III), VO(II), Zr(IV) and UO2(II), with Schiff base derived from 2-hydroxy-5-methylacetophenone and isonicotinic acid hydrazide (HMAIH) have been prepared. The ligand acts as monobasic bidentate, monobasic tridentate and dibasic tridentate depending upon the reaction conditions. The thermal data have been analyzed for the activation energies by Broido's method and obey first order kinetics. The ligand and the complexes have been screened for their antimicrobial activity. (author)

  17. Polymer conjugates of doxorubicin bound through an amide and hydrazone bond: impact of the carrier structure onto synergistic action in the treatment of solid tumours

    Czech Academy of Sciences Publication Activity Database

    Etrych, Tomáš; Šubr, Vladimír; Laga, Richard; Říhová, Blanka; Ulbrich, Karel

    2014-01-01

    Roč. 58, 16 July (2014), s. 1-12. ISSN 0928-0987 R&D Projects: GA ČR GAP301/11/0325; GA MŠk EE2.3.30.0029; GA MŠk(CZ) ED1.1.00/02.0109 Institutional support: RVO:61389013 ; RVO:61388971 Keywords : HPMA copolymer * synergistic effect * doxorubicin Subject RIV: CE - Biochemistry; FD - Oncology ; Hematology (MBU-M) Impact factor: 3.350, year: 2014

  18. A Novel and Expedient Approach to New Thiazoles, Thiazolo[3,2-a]pyridines, Dihydrothiophenes, and Hydrazones Incorporating Thieno[2,3-b]thiophene Moiety

    Directory of Open Access Journals (Sweden)

    Taleb T. Al-Nahary

    2012-04-01

    Full Text Available This paper reports details about the synthesis of a series of novel functionalized symmetrical bis-heterocyclic compounds containing a thieno[2,3-b]thiophene motif. Bis-thiazole derivatives 2, 3a-c and thiazolo[3,2-a]pyridine derivatives 4a-c are achieved. The hitherto unknown dihydrothiophene derivatives 6a-d via bis-pyridimium salt 5 are obtained. Additionally, the novel hydrazonothieno[2,3-b]thiophene derivatives 10a-c are obtained via bis-tosylacetylthieno[2,3-b]thiophene derivative 9. All compounds are characterized by 1H-, 13C-NMR, GCMS, IR, and UV-vis spectrometry. These compounds represent a new class of sulfur and nitrogen containing heterocycles that should also be of interest as new materials.

  19. Palladium-Catalyzed One-Pot Reaction of Hydrazones, Dihaloarenes, and Organoboron Reagents: Synthesis and Cytotoxic Activity of 1,1-Diarylethylene Derivatives.

    Science.gov (United States)

    Roche, Maxime; Salim, Salim Mmadi; Bignon, Jérôme; Levaique, Hélène; Brion, Jean-Daniel; Alami, Mouad; Hamze, Abdallah

    2015-07-01

    A new three-component assembly reaction between N-tosylhydrazones, dihalogenated arenes, and boronic acids or boronate esters was developed, producing highly substituted 1,1-diarylethylenes in good yields. The two C-C bonds formed through this coupling have been catalyzed by a single Pd-catalyst in a one-pot fashion. It is noted that the one-pot pinacol boronate cross-coupling reaction generally provides products in high yields, offers an expansive substrate scope, and can address a broad range of aryl, styrene, vinyl, and heterocyclic olefinic targets. The scope of this one-pot coupling has been also extended to the synthesis of the 1,1-diarylethylene skeleton of the natural product ratanhine. The new compounds were evaluated for their cytotoxic activity, and this allowed the identification of compound 4ab that exhibits excellent antiproliferative activity in the nanomolar concentration range against HCT116 cancer cell lines. PMID:26036279

  20. p-Tolyl 2-O-benzoyl-3-O-benzyl-4,6-O-benzylidene-1-thio-α-l-idopyranoside

    Directory of Open Access Journals (Sweden)

    Graeme J. Gainsford

    2010-07-01

    Full Text Available The title compound, C34H32O6S, is an ido-configured thioglycoside building block for heparan sulfate fragments. It contains disordered tolyl and O-benzyl groups with occupancy ratios of 0.539 (13:0.461 (13 and 0.613 (13:0.387 (13, respectively, as determined from a weakly diffracting crystal. The fused rings adopt chair conformations with the molecules packing into a three-dimensional network via C—H...O and three C—H...π interactions. The former interactions, occuring between molecules related by a twofold axis, define an R22(26 motif.

  1. Structure of enzyme-bound substrates: resonance Raman and kinetic evidence for differential enzyme-substrate contacts in N-(Pentafluoro-benzoyl)glycine dithioacyl and thioacyl papain

    Science.gov (United States)

    Lee, H.; Angus, R. H.; Storer, A. C.; Carey, P. R.

    1989-12-01

    Resonance Raman (RR) spectroscopy is used to probe the structure of the substrate in the substrate-enzyme complex N-pentafluorobenzoyl) glycine (dithioacyl) papain (C 6F 5C(=O) NHCH 2C(=S)S-papain). This system was chosen since the high electron withdrawing capacity of the C 6F 5 group markedly affects electron density of the -NH- moiety which, in turn, is known to change catalytic activity. The RR spectrum of the enzyme-substrate complex is interpreted by reference to the model compound N-(pentafluorobenzoyl) glycine ethyl dithioester (C 6F 5(CO))NHCH 2C(=S)SC 2H 5. The RR spectra of this compound in aqueous or organic solvents can be understood in terms of the known conformational states of N-acylglycine dithioesters. Comparison of model with enzyme-substrate RR spectra shows that the substrate is binding in the active site in a conformer known as conformer B characterized by a small-NHCH 2CS(thiol) torsional angle and close N-to-S (thiol) contact. Kinetic rate-structure correlations are developed involving k3, the rate constant for deacylation, and the strength of the N-to-S (thiol) interaction. N-(Pentafluorobenzoyl) glycine dithioacyl papain fits the rate-structure correlation whereas the corresponding pentafluorobenzoyl glycine thiol intermediate does not. It is proposed that the difference in the size of the CS compared to the CO group brings about a small change in the dithioacyl papain compared to the thiolacyl papain conformation such that enzyme-substrate contacts involving ortho and meta F atoms in the thiol acyl enzyme case are weakened or removed in the case of the dithioacyl papain.

  2. Solvent extraction of hexavalent plutonium with 1-phenyl, 3-methyl, 4-benzoyl pyrazolone-5 (HPMBP) and bi-dentate neutral donors (DBDECMP, DHDECMP and CMPO): synergism and thermodynamics

    International Nuclear Information System (INIS)

    Synergistic extraction of hexavalent plutonium was studied with HPMBP in combination with DBDECMP, DHDECMP or CMPO in benzene medium at various fixed temperatures. The equilibrium constants for the organic phase addition reaction (log Ks) were found to follow the trend in basicity of the neutral donors. Thermodynamic parameters were evaluated and these indicated that organic phase reaction is an addition and not a substitution reaction. Further, the bidentate donors act as monodentates. (orig.)

  3. Synergistic extraction of dioxoplutonium with 1-phenyl, 3-methyl, 4-benzoyl pyrazolone-5(HPMBP) and bi-dentate neutral donors (DBDECMP, DHDECMP and CMPO)

    International Nuclear Information System (INIS)

    Synergistic extraction of plutonyl ion was studied with HPMBP in combination with (bidentate neutral donors) DBDECMP, DHDECMP or CMPO using benzene as the diluent. The species extracted was established to be, PuO2(PMBP)2.S. Equilibrium constants (log Ks) of the organic phase addition reaction were found to follow the order of basicity (Kh) of the neutral donors. (author). 2 refs., 3 figs., 1 tab

  4. Solvent extraction of lanthanum(III), europium(III) and lutetium(III) with fluorinated 1-phenyl-3-methyl-4-benzoyl-5-pyrazolones into chloroform.

    Science.gov (United States)

    Saleh, M I; Ahmad, M; Darus, H

    1990-07-01

    A series of chelating reagents, 1-phenyl-3-methyl-4-(2-fluorobenzoyl)-5-pyrazolone, 1-phenyl-3-methyl-4-(3-fluorobenzoyl)-5-pyrazolone and 1-phenyl-3-methyl-4-(4-fluorobenzoyl)-5-pyrazolone, has been synthesized. The extraction of Ln(III), (Ln = La, Eu and Lu) into chloroform with these reagents at 30 +/- 1 degrees has been studied. The composition of the complexes extracted has been determined by the slope method, and the extraction constants K(ex), were measured. The presence of the fluorine atom in the reagents does not make the K(ex), values much different from those obtained with the parent pyrazolone. PMID:18965016

  5. Solvent extraction of lanthanum(III), europium(III) and lutetium(III) with fluorinated 1-phenyl-3-methyl-4-benzoyl-5-pyrazolones into chloroform

    International Nuclear Information System (INIS)

    A series of chelating reagents, 1-phenyl-3-methyl-4-(2-fluorobenzoyl)-5-pyrazolone, 1-phenyl-3-methyl-4-(3-fluorobenzoyl)-5-purazolone and 1-phenyl-3-methyl-4-(4-fluorobenzoyl)-5-pyrazolone, has been synthesized. The extraction of Ln(III), (Ln = La, Eu and Lu) into chloroform with these reagents at 30±10 has been studied. The composition of the complexes extracted has been determined by the slope method, and the extraction constants Kex, were measured. The presence of the fluorine atom in the reagents does not make the Kex values much different from those obtained with the parent pyrazolone. (author)

  6. 5-Benzoyl-4-hydroxy-6-(4-nitrophenyl-4-trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Feng-Ling Yang

    2009-01-01

    Full Text Available The asymmetric unit of the title compound, C18H14F3N3O5·H2O, contains two independent formula units. The two heterocyclic molecules differ in the orientations of the benzoylphenyl group with respect to the tetrahydropyrimidine ring [C—C—C—C torsion angles of 64.5 (3 and 67.1 (3°]. In both molecules the pyrimidine ring adopts a half-chair conformation. The molecules are linked into a two-dimensional network parallel to (001 by N—H...O and O—H...O hydrogen bonds.

  7. Structure and spectroscopic properties of ruthenium(II) bipyridyl N-benzoyl-N'-(1,10-phenanthrolin-5-Yl)-thiourea

    International Nuclear Information System (INIS)

    Ruthenium bipyridyl incorporating phenanthroline with thiourea molecules, [Ru(bpy)2(Phen-BT)](PF6)2], has been synthesized and characterized by spectroscopic and electrochemical techniques. The infrared spectra of the complex shows the characteristics stretching frequencies for N-H at 3646 and 3585 cm−1, ν(C-N)phen 1426 cm−1, ν(C=O) 1675 cm−1, ν(C=S) 1246 cm−1, ν(C-H)aromatic 3353-3086 cm−1, ν(C-N)aliphatic 1169-1026 cm−1, ν(C-H)bend 764 cm−1 and ν(PF6−)free 842 cm−1. The complex reveals two π→π* absorption bands at 237 (ε=26,302) and 286 nm (ε=36,848), which were assigned to the phenanthroline and bipyridyl moieties, respectively. A slightly broad and low energy band in the UV-vis spectrum at 450 nm (ε=7,209) of the complex was assigned to a MLCT transition. Besides, the complex also exhibits an emission band at 615 nm that arises from an excitation with a 440 nm light energy. The cyclic voltammetry of the complex shows an oxidation potential at +1.305 V vs. SCE that corresponds to the formal oxidation of Ru(II) to Ru(III)

  8. Studies on Synthesis of Some Novel Heterocyclic Chalcone, Pyrazoline, Pyrimidine - 2 - One, Pyrimidine - 2 - Thione, para-Acetanilide Sulphonyl and Benzoyl Derivatives and their Antimicrobial Activity

    OpenAIRE

    Mistry, Rakesh N.; K. R. Desai

    2005-01-01

    1, 2 - Dichloro benzene on chlorosulphonation by chlorosulphonic acid gives 1, 2 - [dichloro] - benzene sulphonyl chloride which on condensation with p –amino acetophenone gives 1-[acetyl] - 1’ , 2’ - [dichloro] - dibenz sulphonamide derivative. This derivative undergo condensation with 2,4- dichloro benzaldehyde gives 1- [3” - (sub. phenyl) - 2” - propene - 1” - one] - 1’ , 2’ - [dichloro] - dibenz sulphonamide derivative which on reaction with 99% hydrazine hydrate and glacial acetic acid g...

  9. 1-Benzoyl-3-[3-cyano-8-methyl-4-(1-methyl-1H-pyrrol-2-yl-5,6,7,8-tetrahydroquinolin-2-yl]thiourea

    Directory of Open Access Journals (Sweden)

    Abdullah M. Asiri

    2011-09-01

    Full Text Available In the N-substituted benzoylthiourea, C24H23N5OS, the benzoylthiourea unit is non-planar (r.m.s. deviation = 0.126 Å. The aliphatic part of the tetrahydroquinoline fused-ring system is disordered over two positions in a 0.592 (5:0.408 (5 ratio. The pyridine and pyrrole rings are twisted by 55.2 (1° in order to avoid crowding of their respective substituents. Pairs of molecules are linked by N—H...N hydrogen bonds, forming centrosymmetric dimers. Furthermore, an intramolecular N—H...O hydrogen bond stabilizes the molecular conformation.

  10. Structure and spectroscopic properties of ruthenium(II) bipyridyl N-benzoyl-N'-(1,10-phenanthrolin-5-Yl)-thiourea

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Siew San [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor (Malaysia); Kassim, Mohammad B. [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor (Malaysia)

    2015-09-25

    Ruthenium bipyridyl incorporating phenanthroline with thiourea molecules, [Ru(bpy){sub 2}(Phen-BT)](PF{sub 6}){sub 2}], has been synthesized and characterized by spectroscopic and electrochemical techniques. The infrared spectra of the complex shows the characteristics stretching frequencies for N-H at 3646 and 3585 cm{sup −1}, ν(C-N){sub phen} 1426 cm{sup −1}, ν(C=O) 1675 cm{sup −1}, ν(C=S) 1246 cm{sup −1}, ν(C-H){sub aromatic} 3353-3086 cm{sup −1}, ν(C-N){sub aliphatic} 1169-1026 cm{sup −1}, ν(C-H){sub bend} 764 cm{sup −1} and ν(PF{sub 6}{sup −}){sub free} 842 cm{sup −1}. The complex reveals two π→π* absorption bands at 237 (ε=26,302) and 286 nm (ε=36,848), which were assigned to the phenanthroline and bipyridyl moieties, respectively. A slightly broad and low energy band in the UV-vis spectrum at 450 nm (ε=7,209) of the complex was assigned to a MLCT transition. Besides, the complex also exhibits an emission band at 615 nm that arises from an excitation with a 440 nm light energy. The cyclic voltammetry of the complex shows an oxidation potential at +1.305 V vs. SCE that corresponds to the formal oxidation of Ru(II) to Ru(III)

  11. Synthesis and X-ray crystal structure determination of N-p-methylphenyl-4-benzoyl-3,4-diphenyl-2-azetidinone

    International Nuclear Information System (INIS)

    The title compound, C29H23NO2, has been characterized by single-crystal X-ray diffraction at two different temperatures (303 K and 120 K) and wavelengths (MoKα and CuKα). The non-centrosymmetric hexagonal crystal structure contains four-membered planar β-lactam ring with an unusually long C-C bond. The β-lactam ring is almost planar.

  12. Rearrangement of 11-Hydroxy-11-(2-naphthyl)-3,4:8,9-dibenzobicyclo [4.4.1]undeca-3,8-diene-2,2,5,5,7,7,10,10-d_8

    OpenAIRE

    Isobe, Shin-ichiro; Thiemann, Thies; Sawada, Tsuyoshi; Yonemitsu, Tadashi; Mataka, Shuntaro

    2000-01-01

    The preparation of a novel deuterated [3.3]orthocyclophane-alcohol is described. The rearrangement of the orthocyclophane alcohol leads to a dibenzo-annelated bromomethyldecaline. The deuterium labels provide a good indication of the mechanism that is underlying this reaction.

  13. Synthesis of 2-(6' methoxy-2'-naphthyl) Propylaldehyde Thiosemicarbazones(dl)%萘丙醛缩硫代氨基脲类外消旋体的合成

    Institute of Scientific and Technical Information of China (English)

    程石泉; 乌力吉木仁; 杨国宏; 王佩珠

    1988-01-01

    @@萘普生[(+)6'-Methoxy-2'-methyl(2-Naphthalene)acetic acid]作为一种强效的解热、抗炎、镇痛药物,属于非甾体类化合物。1968年美国Syntex公司等首先报道了它的合成方法,《医药工业》曾作了详细综述[1]。目前已用于临床,国内也已批量生产。 从五十年代起,人们就已经知道:缩氨基硫脲具有抗结核[2]、治疗麻风病[3]等作用,同时也发现它产生一些副作用[4],随后,人们又对缩氨硫脲和其他药物联合用药进行探索[5]获得良好治疗效果。据此,我们用2-(6'-甲氧基-2'-萘基)丙醛为载体,分别与羟氨、苯基氨基脲、硫代氨基脲在适当条件下缩合,制得萘丙醛羟胺[Ⅰ]、萘丙醛缩苯基氨基脲[Ⅱ]和萘丙醛缩硫代氨基脲三个新化合物,迄今为止,未见文献报道。我们用氨基脲进行多次实验,均未获得成功。上述制得产物[Ⅰ-Ⅲ],试图找到一种具有新的生理活性的新药。

  14. Synthesis and Curing Properties of a Novel Novolac Curing Agent Containing Naphthyl and Dicyclopentadiene Moieties%新型含萘环/环戊二烯环结构固化剂的合成及性能

    Institute of Scientific and Technical Information of China (English)

    任华; 孙建中; 吴斌杰; 周其云

    2007-01-01

    A novel novolac curing agent containing both naphthalene and dicyclopentadiene (DCPD) moieties was prepared to produce a highly heat-resistant cured polymer network. The chemical structure was characterized using Fourier transform infrared spectroscopy, nuclear magnetic resonance, mass spectrometry, and gel permeation chromatography analyses. The thermal properties of the resulting polymer from diglycidyl ether of bisphenol A epoxy resin cured with the novel curing agent were evaluated using dynamic mechanical thermal analysis and thermogravimetric analysis. Compared with the conventional curing agent, the resulting polymer cured with naphthalene/DCPD navolac shows considerable improvement in heat resistant properties such as higher glass transition temperature (Tg) and thermal stability. The result also shows better moisture resistance because of the hydrophobic nature of naphthalene/DCPD structure.

  15. Synthesis and antitumor activity of derivatives of 23-hydroxybetulinic acid

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A series of natural product 23-hydroxybetulinic acid derivatives were prepared. In the preparation of mono-O-benzoyl ester derivative, it was observed that benzoyl group migrated from 3-O- to 23-O-position during the detritylation.

  16. Synthesis and Antifungal Activity of Two Hydrazones Derived from Vanillin%两种香兰素腙类化合物的合成及抑菌活性初步研究

    Institute of Scientific and Technical Information of China (English)

    邹怀波; 周蓉; 梁辉; 南建忠

    2011-01-01

    Reactions of vanillin with phenylhydrazine and 4-nitrophenylhydrazine in methanol or acetic acid resulted in the vanillinphenylhydrazone,and vanillin-4-nitrophenylhydrazone, respectively. These products were identified by IR and 1H-NMR.And the preliminary antifungal experiments indicated that these compounds had some antifungal activity against E. coli and S. aureus.%以香兰素为原料,与苯肼和对硝基苯肼缩合得到两种香兰素腙类化合物,其结构经1H-NMR、IR表征.初步的抑菌试验表明,这些化合物对大肠杆菌(Escherichia coli)和金黄色葡萄球菌(Staphylococcus aureus)具有一定的抑菌效果.

  17. Investigation de la synthèse mécanochimique de 1,4-diazines condensées et d'hydrazones d’intérêt pharmaceutique

    OpenAIRE

    Marques de Oliveira, Paulo Filho

    2015-01-01

    L'un des objectifs des industries chimique et pharmaceutique est de développer des procédés verts évitant ou réduisant l'utilisation de solvants. Mais ne pas utiliser de solvant nécessite souvent des catalyseurs métalliques ou autre, ce qui rend les purifications délicates, comme dans le cas des synthèses de chimie fine permettant l'obtention de principes actifs pharmaceutiques. C'est ainsi que la mécanochimie a émergé en tant que voie durable pour la synthèse chimique, y compris dans le cas ...

  18. Experimental and Theoretical Studies on the Functionalization Reactions of 4-Benzoyl-1,5-Diphenyl-1H-Pyrazole-3-Carboxylic Acid and Acid Chloride with 2,3-Diaminopyridine

    Directory of Open Access Journals (Sweden)

    Elif Demir

    2005-03-01

    Full Text Available The 1H-pyrazole-3-carboxylic acid 2 was converted in good yield (69% into the corresponding 1H-pyrazole-3-carboxamide 5 via reaction of the acid chloride 3 with 2,3- diaminopyridine (4. A different product, the 3H-imidazo[4,5-b] pyridine derivative 6, was formed from the reaction of 3 with 4 and base in benzene for 5 hours. The structures of the synthesized compounds were determined spectroscopically. The mechanism of the reaction between 3 and 4 was examined theoretically.

  19. Part 1: Method Development for the Analysis of Polyamines by Derivatives with Benzoyl Chloride by HPLC Tandem Mass Spectrometry Part 2: Detection of Volatile Organic Compound Tracers in Human Breath

    OpenAIRE

    Jenny Kim

    2015-01-01

    Part 1: Development and validation of an analytical method by liquid chromatography-tandem mass spectrometry to detect putrescine, cadaverine, spermidine, spermine, n8-acetylspermidine, and n1-acetylspermine as benzyl amide derivatives in biological samples were completed. The derivatization conditions were optimized for all PAs, and method validation was completed for putrescine (PUT) and spermidine (SPD) using isotope dilution techniques. The method exhibited: high accuracy (

  20. Labelling and quality control of somatostatin analogues with 99mTc

    International Nuclear Information System (INIS)

    Techniques and methodologies for labelling peptides with 99mTc and methods for their purification, chemical, radiochemical and biological controls were evaluated. With the purpose of gaining experience, labelling with 125I was also studied. RC-160 was labelled with 125I using iodogen as well as chloramine-T method. Higher yields were obtained with chloramine-T method (60%), rendering 125I-peptide with 98% of radiochemical purity, with specific activity of 240 μCi/μg - 274 μCi/μg. The product was stable for five weeks (at -20 deg. C). For somatostatin receptors studies rat brain cortex membrane was prepared. Maximum binding capacity was 24.7% and Kaff for the binding of RC-160 to receptor was estimated as 2.0x1010 M-1. Other peptides as β-(2-Naphthyl)-DAla-Cys-Tyr-DTrp-Lys-Val-Cys-Thr amide (N-9642, Σ) and mouse epidermal growth factor (mEGF) were also labelled by means of limiting chloramine-T method. In case of mEGF the availability of membrane receptors allowed us to experiment in mice as well as in vitro. The reaction yields were up to 60% and 70% respectively. Biodistribution of 125I-mEGF in a mouse with adenoma demonstrated preferential uptake in tumour (21,7% injected dose). The radioimmunoassay system gave 39% maximum binding (MB) and 50% displacement (ED50) for 10 ng/mL unlabelled mEGF. Direct method and BFC's for labelling peptides with 99mTc were investigated and purification and quality controls studies were performed by TLC, HPLC (UV and gamma detection). RC-160 was labelled by a direct method using sodium dithionite as reducing agent with radiochemical purity >95%. The product was stable up to six hours (at RT). Considerable adsorption problems were observed. Biological behavior was in accordance with the compounds' lipophilicity. The synthesis of TOC conjugates with HYNIC as BFC was done with 45%±5% (n=3) yield. Labelling of HYNIC-TOC with tricine as co-ligand was conducted with up to 90% yield. Studies of RC-160 labelling using 99m

  1. Non-specific esterases and esterproteases in masticatory muscles from the muscular dystrophic mouse

    DEFF Research Database (Denmark)

    Kirkeby, S; Moe, D; Vilmann, H

    1989-01-01

    With the aid of histochemical and electrophoretic techniques activities for esterase and esterprotease were investigated in the digastric and masseter muscles from normal and dystrophic mice. The substrates used were alpha-naphthyl acetate and N-acetyl-L-alanine alpha-naphthyl ester. According to...

  2. Effect of surface modification of Grewia optiva fibres on their physicochemical and thermal properties

    Indian Academy of Sciences (India)

    Amar S Singha; Ashvinder K Rana

    2012-12-01

    This paper deals with the surface modification of Grewia optiva fibre through benzoylation and graft copolymerization process. Benzoylation of Grewia optiva fibre has been carried out on mercerized fibre with varying concentrations of benzoyl chloride solution. Graft copolymerization of acrylonitrile (AN) onto Grewia optiva fibre was carried out with ceric ammonium nitrate as the redox initiator in aqueous medium under the influence of microwave radiation. Raw, graft copolymerized and benzoylated fibres were subjected to evaluation of some of their properties like swelling behaviour, moisture absorbance and chemical resistance behaviour. It has been observed that 5% benzoyl chloride treated and graft copolymerized Grewia optiva show more resistance towards moisture, water and chemicals when compared with that of raw fibre. Further morphological, structural changes, thermal stability and crystallinity of raw, graft copolymerized, pretreated and benzoylated fibres have also been studied by SEM, FTIR, TGA and XRD techniques.

  3. Chiral Recognition for the Two Enantiomers of Phenylalanine and Four Amino Acid Derivatives with (S)-Phenylethylamine Derived Nickel(II) Macrocyclic Complex

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Jeong Jae; Ryoo, Jae Jeong [Kyungpook National Univ., Daegu (Korea, Republic of)

    2013-11-15

    The potency of new chiral selector candidate was assessed by this simple chiral discrimination test. This experiment showed that the macrocyclic molecule can be a powerful candidate as a chiral selector to obtain optically pure amino acid or amino acid derivatives, particularly phenylalanine and N-benzoyl-phenylalanine enantiomers from racemic mixtures. This study attempted to use the chiral metal organic framework (MOF), 1, as a good chiral selector candidate for the chiral discrimination of racemic phenylalanine, N-benzoyl-alanine, N-benzoyl-phenylalanine, N-benzoyl-methionine, N-CBZ-alanine. The chiral recognition ability of the chiral macromolecule, was examined by varying the molar ratio of the macromolecule and racemates.

  4. Chiral Recognition for the Two Enantiomers of Phenylalanine and Four Amino Acid Derivatives with (S)-Phenylethylamine Derived Nickel(II) Macrocyclic Complex

    International Nuclear Information System (INIS)

    The potency of new chiral selector candidate was assessed by this simple chiral discrimination test. This experiment showed that the macrocyclic molecule can be a powerful candidate as a chiral selector to obtain optically pure amino acid or amino acid derivatives, particularly phenylalanine and N-benzoyl-phenylalanine enantiomers from racemic mixtures. This study attempted to use the chiral metal organic framework (MOF), 1, as a good chiral selector candidate for the chiral discrimination of racemic phenylalanine, N-benzoyl-alanine, N-benzoyl-phenylalanine, N-benzoyl-methionine, N-CBZ-alanine. The chiral recognition ability of the chiral macromolecule, was examined by varying the molar ratio of the macromolecule and racemates

  5. Novas N-benzoiltiraminas de Swinglea glutinosa (Rutaceae)

    OpenAIRE

    Cristovam do Nascimento Cerqueira; Djalma A. P. dos Santos; Karla da Silva Malaquias; Murilo Marinho de Castro Lima; Maria Fátima das Graças Fernandes da Silva; João Batista Fernandes; Paulo Cezar Vieira

    2012-01-01

    Phytochemical studies of the leaves and fruits have led to the identification of the known amides (E)-N-methyl-cinnamamide, N-benzoyltyramine, N-benzoyl-O-geranyltyramine, N-benzoyl-O-(4-acetoxyl)-geranyltyramine, in addition to the new N-{2-[4-(butoxyl-3-one)phenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxylanal)phenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxyloic)phenyl]ethyl}benzamide, N-benzoyl-O-(4-acetoxyl-6,7-epoxy)-geranyltyramine, N-benzoyl-O-(4-acetoxyl-6,...

  6. Novel N-benzoyltyramines of Swinglea glutinosa (Rutaceae); Novas N-benzoiltiraminas de Swinglea glutinosa (Rutaceae).

    Energy Technology Data Exchange (ETDEWEB)

    Cerqueira, Cristovam do Nascimento; Santos, Djalma A.P. dos; Malaquias, Karla da Silva; Lima, Murilo Marinho de Castro; Silva, Maria Fatima das Gracas Fernandes da; Fernandes, Joao Batista; Vieira, Paulo Cezar, E-mail: dmfs@ufscar.br [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica

    2012-07-01

    Phytochemical studies of the leaves and fruits have led to the identification of the known amides (E)-N-methyl-cinnamamide, N-benzoyltyramine, N-benzoyl-O-geranyl tyramine, N-benzoyl-O-(4-acetoxyl)-geranyl tyramine, in addition to the new N-{l_brace}2-[4-(butoxyl-3-one)phenyl]ethyl{r_brace}benzamide, N-{l_brace}2-[4-(2,3-dihydroxy-2-methyl-butoxylanal)phenyl]ethyl{r_brace}benzamide, N-{l_brace}2-[4-(2,3-dihydroxy-2-methyl-butoxyloic) phenyl]ethyl{r_brace}benzamide, N-benzoyl-O-(4-acetoxyl-6,7-epoxy)-geranyltyramine, N-benzoyl-O-(4-acetoxyl-6,7-dihydroxy)-geranyltyramine and N-benzoyl-O-(6-acetoxyl-4,7-dihydroxy)-geranyltyramine. The isolated compounds clearly point to Swinglea phytochemical affinities with other Aurantioideae species. (author)

  7. Novas N-benzoiltiraminas de Swinglea glutinosa (Rutaceae

    Directory of Open Access Journals (Sweden)

    Cristovam do Nascimento Cerqueira

    2012-01-01

    Full Text Available Phytochemical studies of the leaves and fruits have led to the identification of the known amides (E-N-methyl-cinnamamide, N-benzoyltyramine, N-benzoyl-O-geranyltyramine, N-benzoyl-O-(4-acetoxyl-geranyltyramine, in addition to the new N-{2-[4-(butoxyl-3-onephenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxylanalphenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxyloicphenyl]ethyl}benzamide, N-benzoyl-O-(4-acetoxyl-6,7-epoxy-geranyltyramine, N-benzoyl-O-(4-acetoxyl-6,7-dihydroxy-geranyltyramine and N-benzoyl-O-(6-acetoxyl-4,7-dihydroxy-geranyltyramine. The isolated compounds clearly point to Swinglea phytochemical affinities with other Aurantioideae species.

  8. Novel N-benzoyltyramines of Swinglea glutinosa (Rutaceae)

    International Nuclear Information System (INIS)

    Phytochemical studies of the leaves and fruits have led to the identification of the known amides (E)-N-methyl-cinnamamide, N-benzoyltyramine, N-benzoyl-O-geranyl tyramine, N-benzoyl-O-(4-acetoxyl)-geranyl tyramine, in addition to the new N-{2-[4-(butoxyl-3-one)phenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxylanal)phenyl]ethyl}benzamide, N-{2-[4-(2,3-dihydroxy-2-methyl-butoxyloic) phenyl]ethyl}benzamide, N-benzoyl-O-(4-acetoxyl-6,7-epoxy)-geranyltyramine, N-benzoyl-O-(4-acetoxyl-6,7-dihydroxy)-geranyltyramine and N-benzoyl-O-(6-acetoxyl-4,7-dihydroxy)-geranyltyramine. The isolated compounds clearly point to Swinglea phytochemical affinities with other Aurantioideae species. (author)

  9. Improving Grubbs' II type ruthenium catalysts by appropriately modifying the N-heterocyclic carbene ligand.

    Science.gov (United States)

    Vieille-Petit, Ludovic; Luan, Xinjun; Gatti, Michele; Blumentritt, Sascha; Linden, Anthony; Clavier, Hervé; Nolan, Steven P; Dorta, Reto

    2009-07-01

    The introduction of N-heterocyclic carbene ligands that incorporate correctly substituted naphthyl side chains leads to increased activity and stability in second generation ruthenium metathesis catalysts. PMID:19557281

  10. A Systematic Study of the Effects of Naphthalene and Anthracene Substitution on the Properties of PPV Derivative Conjugated Systems

    OpenAIRE

    Lynch, Patrick; O'Neill, Luke; Bradley, David; Byrne, Hugh; McNamara, Mary

    2007-01-01

    The systematic synthesis of poly(phenylvinylene) (PPV) derivatives by the Wittig-Horner reaction is reported. The phenyl units of the PPV structure are methodically substituted by naphthyl and anthryl units to form a homologous series of structures. The 2,6 attachment of the vinylene linkage on the anthryl ring provides novel structures that have not been reported before due to their synthetic inaccessibility. The introduction of naphthyl units results in a hypsochromatic shift in the absorpt...

  11. The impact of isatin derivatives on antibiotic production by Streptomyces hygroscopicus CH-7

    Directory of Open Access Journals (Sweden)

    Ćirić Jovan T.

    2016-01-01

    Full Text Available The effect of isatin derivatives as a nitrogen source on antibiotic (Hexaene H-85 and Azalomycine B production by Streptomyces hygroscopicus CH-7 was studied. Isatin-3-hydrazone, 5-chloroisatin-3-hydrazone, isatin-3-tosylhydrazone, 5-chloroisatin-3-tosylhydrazone, isatin-3-(4`-hidroxybenzoilhydrazone and 5-chloroisatin-3-(4`-hidroxybenzoilhydrazone were synthesized in a crude glycerol, obtained during the biodiesel production from edible sunflower oil. The highest concentration of Hexaene H-85 is achieved with 5-chloroisatin-3-hydrazone (197 mg/cm3 in medium, while isatin-3-hydrazone has a greatest impact on Azalomycine B production (72 μg/cm3. [Projekat Ministarstva nauke Republike Srbije, br. III 45001

  12. The impact of isatin derivatives on antibiotic production by Streptomyces hygroscopicus CH-7

    OpenAIRE

    Ćirić Jovan T.; Konstantinović Sandra S.; Ilić Slavica B.; Gojgić-Cvijović Gordana; Savić Dragiša S.; Veljković Vlada B.

    2016-01-01

    The effect of isatin derivatives as a nitrogen source on antibiotic (Hexaene H-85 and Azalomycine B) production by Streptomyces hygroscopicus CH-7 was studied. Isatin-3-hydrazone, 5-chloroisatin-3-hydrazone, isatin-3-tosylhydrazone, 5-chloroisatin-3-tosylhydrazone, isatin-3-(4`-hidroxy)benzoilhydrazone and 5-chloroisatin-3-(4`-hidroxy)benzoilhydrazone were synthesized in a crude glycerol, obtained during the biodiesel production from edible sunflower oil. ...

  13. Asymmetrische Synthese neuer planar- und zentral-chiraler Ferrocenylliganden

    OpenAIRE

    Klumpen, Thomas

    2003-01-01

    In this thesis we describe the enantioselective synthesis of mono- and di-ortho-substituted ferrocenyl diketones via our SAMP/RAMP-hydrazone method. Keystep is the stepwise diastereoselective ortho-metalation of 1,1'-bisbenzoylferrocene-bis-SAMP-hydrazone followed by trapping of various types of electrophiles. Within our studies we demonstrate the broad applicability of this method by using alkyl-, silyl-, phosphin- and sulfur electrophiles. We obtained the desired products in very good yield...

  14. Microwave-Assisted Rapid Access to Bio-active Heterocycles: Synthesis of 1,3,4-Oxadiazoles, 1,3,4-Thiadiazoles, 1,3-Dioxanes, Pyrazoles, Hydrazones and 3,4-Dihydropyrimidin-2(1H)-ones under Benign Conditions

    Science.gov (United States)

    Green chemistry is a rapidly developing new field that provides us a proactive avenue for the sustainable development of future science and technologies.1 It emphasis the use of highly efficient and environmental benign synthetic protocols to deliver bio-active heterocycles, acc...

  15. Two mixed-ligand lanthanide–hydrazone complexes: [Pr(NCS3(pbh2]·H2O and [Nd(NCS(NO3(pbh2(H2O]NO3·2.33H2O [pbh is N′-(pyridin-2-ylmethylidenebenzohydrazide, C13H11N3O

    Directory of Open Access Journals (Sweden)

    Damianos G. Paschalidis

    2016-02-01

    Full Text Available The gel-mediated syntheses and crystal structures of [N′-(pyridin-2-ylmethylidene-κNbenzohydrazide-κ2N′,O]tris(thiocyanato-κNpraseodymium(III monohydrate, [Pr(NCS3(C13H11N3O2]·H2O, (I, and aqua(nitrato-κ2O,O′[N′-(pyridin-2-ylmethylidene-κNbenzohydrazide-κ2N′,O](thiocyanato-κNneodymium(III nitrate 2.33-hydrate, [Nd(NCS(NO3(C13H11N3O2(H2O]NO3·2.33H2O, (II, are reported. The Pr3+ ion in (I is coordinated by two N,N,O-tridentate N′-(pyridin-2-ylmethylidenebenzohydrazide (pbh ligands and three N-bonded thiocyanate ions to generate an irregular PrN7O2 coordination polyhedron. The Nd3+ ion in (II is coordinated by two N,N,O-tridentate pbh ligands, an N-bonded thiocyanate ion, a bidentate nitrate ion and a water molecule to generate a distorted NdN5O5 bicapped square antiprism. The crystal structures of (I and (II feature numerous hydrogen bonds, which lead to the formation of three-dimensional networks in each case.

  16. Synthesis of 1-O-Acetyl-2,3,5-Tri-O- Benzoyl-β-D-Ribofuranose%1-O-乙酰基-2,3,5-三-O-苯甲酰基-β-D-呋喃核糖的合成

    Institute of Scientific and Technical Information of China (English)

    陈敖; 柏凤飞; 宋帅娟; 陈小琴; 陆琴亚; 黄荷香

    2009-01-01

    @@ 前言 核苷类药物是抗病毒、抗肿瘤药物研究的重点内容之一,目前已经有多个核苷类药物上市或处于各研究阶段[1].1-O-乙酰基-2,3,5-三-O-苯甲酰基-β-D-呋喃核糖(1)可以用来合成多种核苷类药物,例如Clofarabine、Azacitidine等,市场前景广阔.

  17. Crystallographic and computational studies on 4-phenyl-N-(beta-D-glucopyranosyl)-1H-1,2,3-triazole-1-acetamide, an inhibitor of glycogen phosphorylase: comparison with alpha-D-glucose, N-acetyl-beta-D-glucopyranosylamine and N-benzoyl-N'-beta-D-glucopyranosyl urea binding.

    Science.gov (United States)

    Alexacou, Kyra-Melinda; Hayes, Joseph M; Tiraidis, Costas; Zographos, Spyros E; Leonidas, Demetres D; Chrysina, Evangelia D; Archontis, Georgios; Oikonomakos, Nikos G; Paul, Jashuva V; Varghese, Babu; Loganathan, Duraikkannu

    2008-05-15

    4-Phenyl-N-(beta-D-glucopyranosyl)-1H-1,2,3-triazole-1-acetamide (glucosyltriazolylacetamide) has been studied in kinetic and crystallographic experiments with glycogen phosphorylase b (GPb), in an effort to utilize its potential as a lead for the design of potent antihyperglycaemic agents. Docking and molecular dynamics (MD) calculations have been used to monitor more closely the binding modes in operation and compare the results with experiment. Kinetic experiments in the direction of glycogen synthesis showed that glucosyltriazolylacetamide is a better inhibitor (K(i) = 0.18 mM) than the parent compound alpha-D-glucose (K(i) = 1.7 mM) or beta-D-glucose (K(i) = 7.4 mM) but less potent inhibitor than the lead compound N-acetyl-beta-D-glucopyranosylamine (K(i) = 32 microM). To elucidate the molecular basis underlying the inhibition of the newly identified compound, we determined the structure of GPb in complex with glucosyltriazolylacetamide at 100 K to 1.88 A resolution, and the structure of the compound in the free form. Glucosyltriazolylacetamide is accommodated in the catalytic site of the enzyme and the glucopyranose interacts in a manner similar to that observed in the GPb-alpha-D-glucose complex, while the substituent group in the beta-position of the C1 atom makes additional hydrogen bonding and van der Waals interactions to the protein. A bifurcated donor type hydrogen bonding involving O3H, N3, and N4 is seen as an important structural motif strengthening the binding of glucosyltriazolylacetamide with GP which necessitated change in the torsion about C8-N2 bond by about 62 degrees going from its free to the complex form with GPb. On binding to GP, glucosyltriazolylacetamide induces significant conformational changes in the vicinity of this site. Specifically, the 280s loop (residues 282-288) shifts 0.7 to 3.1 A (CA atoms) to accommodate glucosyltriazolylacetamide. These conformational changes do not lead to increased contacts between the inhibitor and the protein that would improve ligand binding compared with the lead compound. In the molecular modeling calculations, the GOLD docking runs with and without the crystallographic ordered cavity waters using the GoldScore scoring function, and without cavity waters using the ChemScore scoring function successfully reproduced the crystallographic binding conformation. However, the GLIDE docking calculations both with (GLIDE XP) and without (GLIDE SP and XP) the cavity water molecules were, impressively, further able to accurately reproduce the finer details of the GPb-glucosyltriazolylacetamide complex structure. The importance of cavity waters in flexible receptor MD calculations compared to "rigid" (docking) is analyzed and highlighted, while in the MD itself very little conformational flexibility of the glucosyltriazolylacetamide ligand was observed over the time scale of the simulations. PMID:18041758

  18. Photorelease of phosphates: Mild methods for protecting phosphate derivatives

    Directory of Open Access Journals (Sweden)

    Sanjeewa N. Senadheera

    2014-08-01

    Full Text Available We have developed a new photoremovable protecting group for caging phosphates in the near UV. Diethyl 2-(4-hydroxy-1-naphthyl-2-oxoethyl phosphate (14a quantitatively releases diethyl phosphate upon irradiation in aq MeOH or aq MeCN at 350 nm, with quantum efficiencies ranging from 0.021 to 0.067 depending on the solvent composition. The deprotection reactions originate from the triplet excited state, are robust under ambient conditions and can be carried on to 100% conversion. Similar results were found with diethyl 2-(4-methoxy-1-naphthyl-2-oxoethyl phosphate (14b, although it was significantly less efficient compared with 14a. A key step in the deprotection reaction in aq MeOH is considered to be a Favorskii rearrangement of the naphthyl ketone motif of 14a,b to naphthylacetate esters 25 and 26. Disruption of the ketone-naphthyl ring conjugation significantly shifts the photoproduct absorption away from the effective incident wavelength for decaging of 14, driving the reaction to completion. The Favorskii rearrangement does not occur in aqueous acetonitrile although diethyl phosphate is released. Other substitution patterns on the naphthyl or quinolin-5-yl core, such as the 2,6-naphthyl 10 or 8-benzyloxyquinolin-5-yl 24 platforms, also do not rearrange by aryl migration upon photolysis and, therefore, do not proceed to completion. The 2,6-naphthyl ketone platform instead remains intact whereas the quinolin-5-yl ketone fragments to a much more complex, highly absorbing reaction mixture that competes for the incident light.

  19. ChinAfrica briefly introduces the latest Chinese Government regulations

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    @@ Flour Additives Banned Two food additives, benzoyl peroxide and calcium peroxide, are prohibited from flour production starting May I, according to a statement issued by China's Ministry of Health on March 1.

  20. Rosacea

    Science.gov (United States)

    ... the face in winter with a scarf or mask. Avoid facial products with alcohol or other skin irritants (astringents, ... makeup helps to hide redness. Cool compresses, gel masks, and central face massage may be of some benefit. Benzoyl peroxide ...

  1. Antibody-Catalyzed Degradation of Cocaine

    Science.gov (United States)

    Landry, Donald W.; Zhao, Kang; Yang, Ginger X.-Q.; Glickman, Michael; Georgiadis, Taxiarchis M.

    1993-03-01

    Immunization with a phosphonate monoester transition-state analog of cocaine provided monoclonal antibodies capable of catalyzing the hydrolysis of the cocaine benzoyl ester group. An assay for the degradation of radiolabeled cocaine identified active enzymes. Benzoyl esterolysis yields ecgonine methyl ester and benzoic acid, fragments devoid of cocaine's stimulant activity. Passive immunization with such an artificial enzyme could provide a treatment for dependence by blunting reinforcement.

  2. Lanthanide nitrates as Lewis acids in the one-pot synthesis of 1,2,4-oxadiazole derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Vale, Juliana A.; Faustino, Wagner M., E-mail: julianadqf@yahoo.com.br [Departamento de Quimica, Universidade Federal da Paraiba, Joao Pessoa, PB (Brazil); Zampieri, Davila de S.; Moran, Paulo J.S.; Rodrigues, Jose A.R. [Instituto de Quimica, Universidade Estadual de Campinas, SP (Brazil); Sa, Gilberto F. de [Departamento de Quimica Fundamental, CCEN, Universidade Federal de Pernambuco, Recife, PE (Brazil)

    2012-08-15

    In this work we report the use of lanthanide nitrates [Ln(NO{sub 3}){sub 3}] acting as catalyst in direct one pot synthesis of 3-benzoyl- and 3-acetyl-1,2,4-oxadiazoles derivatives from ketones, nitriles and nitric acid. This is the first example of one-pot synthesis of benzoyl- and acetyl 1,2,4-oxadiazoles derivatives preparation using acetophenones derivates with electron-donator groups. (author)

  3. Reaction Mechanism for Cocaine Esterase-Catalyzed Hydrolyses of (+)- and (−)-Cocaine: Unexpected Common Rate-Determining Step

    OpenAIRE

    Liu, JunJun; Zhao, Xinyun; Yang, Wenchao; Zhan, Chang-Guo

    2011-01-01

    First-principles quantum mechanical/molecular mechanical (QM/MM)-free energy (FE) calculations have been performed to examine catalytic mechanism for cocaine esterase (CocE)-catalyzed hydrolysis of (+)-cocaine in comparison with CocE-catalyzed hydrolysis of (−)-cocaine. It has been shown that the acylation of (+)-cocaine consists of nucleophilic attack of hydroxyl group of Ser117 on carbonyl carbon of (+)-cocaine benzoyl ester and the dissociation of (+)-cocaine benzoyl ester. The first react...

  4. a -Oxo Ketene Dithioacetals Chemistry-A Facile Route to the Synthesis of Fused Heterocyclic Compounds

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The fused heterocyclic compounds 2 : imidazo [1,2-a] pyridine 2a-c and pyrido [1,2-a] pyrimidine 2d were obtained from the reaction of a -cinnamoyl ketene dibenzylthio acetals 1 with diamine. When a -cinnamoyl -a '-benzoyl ketene N, N-acetals 3a-b were treated by t-BuONa/t-BuOH solution, 8- benzoyl-pyrido[1,2-a] pyrimidine 4 was produced.

  5. New iridoids from the fruits of Crescentia cujete.

    Science.gov (United States)

    Wang, Gang; Yin, Wei; Zhou, Zhong-Yu; Hsieh, Kun-Lung; Liu, Ji-Kai

    2010-09-01

    Four new 11-nor-iridoids, 6-O-p-hydroxybenzoyl-10-deoxyeucommiol (1), 6-O-benzoyl-10-deoxyeucommiol (2), 6-O-benzoyl-dihydrocatalpolgenin (a mixture of 3 and 4), as well as two known iridoids, ningpogenin (5) and 6-O-p-hydroxybenzoylaucubin (6), were isolated from the fruits of Crescentia cujete Linn. The structures of these compounds were established on the basis of spectroscopic analysis. PMID:20839124

  6. The chemical synthesis of Leishmania donovani phosphoglycan via polycondensation of a glycobiosyl hydrogenphosphonate monomer.

    Science.gov (United States)

    Nikolaev, A V; Chudek, J A; Ferguson, M A

    1995-08-11

    A polycondensation of 2,3,6-tri-O-benzoyl-4-O-(2,3,4-tri-O-benzoyl-beta-D-galactopyranosyl)-al pha-D-mannopyranosyl hydrogenphosphonate in the presence of trimethylacetyl chloride has been used to synthesize a linear poly[beta-D-galactopyranosyl-(1-->4)-alpha-D-mannopyranosyl phosphate] representing the phosphoglycan part of the lipophosphoglycan from Leishmania donovani. PMID:7497476

  7. Penentuan Derajat Grafting Dan Fraksi Gel Dari Polipropilena Terdegradasi Yang Difungsionalisasikan Dengan Maleat Anhidrida

    OpenAIRE

    Hidayani, Tengku Rachmi

    2011-01-01

    A research has been done about determination grafting degree and gel fraction on functionalization of degraded polypropylene with maleic anhydride. Degradation reaction is done with reactive processing technique in internal mixer on temperature 170 o C. Composition of polypropylene : benzoyl peroxide which is 90% : 10%. Grafting reaction is done on temperature 160oC. Composition of degraded polypropylene : maleic anhydride : benzoyl peroxide which is : (95%:3%:2%), (92%:6%:2%), (89%:9%:2%), (...

  8. Dual fluorescence of naphthylamines in alkaline aqueous solution

    Science.gov (United States)

    Ma, Li-Hua; Wen, Zhen-Chang; Lin, Li-Rong; Jiang, Yun-Bao

    2001-10-01

    Dual fluorescence was observed with N-(1-naphthyl)aminoacetate (1-NAA) in aqueous solution of pH 13.0 in the presence of cationic surfactants, cetyltrimethylammonium bromide (CTAB) and chloride (CTAC), below and after the critical micelle concentration (CMC). Similar dual fluorescence was also found with 1- and 2-naphthylamine (1-NA, 2-NA), N-(2-naphthyl)aminoacetate (2-NAA) and (1-naphthyl)ethylenediamine (1-NEDA), in the presence and absence of the cationic surfactants, but not with N, N-disubstituted 1- and 2-NAs. We concluded that the dual fluorescence was due to the excited-state deprotonation of the amino group in these NAs. The p Ka*s of the dual fluorescent NAs were estimated to be around 14 from the dual fluorescence pH titrations. No clear correlation was found for p Ka* with the amino substitution and the presence of cationic micelle.

  9. Synthesis, characterization and biological studies of 1,7- dinaphthyl heptanoids and their metal chelates

    OpenAIRE

    S. Sindhu; Seena Thomachan; V D John

    2015-01-01

    The present investigation includes the synthesis, characterization, antitumour and antimicrobial activities of three new curcuminoid analogues and their metal chelates. Curcuminoid analogues and their metal chelates have great ability to act as antitumour and antimicrobial agents which motivated us and lead to this present work. The new curcuminoid analogues namely 1,7-di(1-naphthyl)-1,6-heptadiene-3,5-dione (1a), 1,7-di(2-methoxy 1-naphthyl)-1,6-heptadiene-3,5-dione (1b), 1,7-di(2-hydroxy ...

  10. Carboxylic ester hydrolases in mitochondria from rat skeletal muscle

    DEFF Research Database (Denmark)

    Kirkeby, S; Moe, D; Zelander, T

    1990-01-01

    organophosphate and organomercury. The activity of the indoxyl acetate esterases was enhanced by the non-ionic detergents Tween-40 and Lubrol. After freezing, thawing and high speed centrifugation most of the alpha-naphthyl acetate splitting enzymes were found in the supernatant, indicating that the enzymes are......A mitochondrial pellet, prepared from rat skeletal muscle, contained a number of carboxylic ester hydrolase isoenzymes. The esterases which split alpha-naphthyl acetate were organophosphate sensitive, whereas two out of three indoxyl acetate hydrolysing enzymes were resistant to both...

  11. Synthesis of some novel hydrazono acyclic nucleoside analogues

    Directory of Open Access Journals (Sweden)

    Mohammad N. Soltani Rad

    2010-05-01

    Full Text Available The syntheses of novel hydrazono acyclic nucleosides similar to miconazole scaffolds are described. In this series of acyclic nucleosides, pyrimidine as well as purine and other azole derivatives replaced the imidazole function in miconazole and the ether group was replaced with a hydrazone moiety using phenylhydrazine. To interpret the dominant formation of (E-hydrazone derivatives rather than (Z-isomers, PM3 semiempirical quantum mechanic calculations were carried out which indicated that the (E-isomers had the lower heats of formation.

  12. Eficácia da combinação tópica de peróxido de benzoíla 5% e clindamicina 1% para o tratamento da hipomelanose macular progressiva: um estudo randomizado, duplo-cego, placebo-controlado Efficacy of topical combination of benzoyl peroxide 5% and clindamycin 1% for the treatment of progressive macular hypomelanosis: a randomized, doubleblind, placebo-controlled trial

    OpenAIRE

    Jussamara Brito Santos; Olga Laura Sena Almeida; Lorena Marçal da Silva; Enio Ribeiro Maynard Barreto

    2011-01-01

    FUNDAMENTOS: A hipomelanose macular progressiva é uma dermatose sem etiologia definida. Não há consenso ou medicação de primeira linha para o seu tratamento e os tratamentos utilizados são pouco eficazes. OBJETIVO: Avaliar a eficácia terapêutica da combinação tópica de peróxido de benzoíla 5% e clindamicina 1% associada à exposição solar para o tratamento da hipomelanose macular progressiva. MATERIAIS E MÉTODOS: Trata-se de um estudo randomizado, duplo-cego, placebo-controlado, no qual os pac...

  13. New ionic polyiodo benzene derivatives useful as X-ray contrast media

    International Nuclear Information System (INIS)

    New ionic polyiodo benzene derivatives are described for use as X-ray contrast media. The basic structure of these compounds has two trio-iodo-benzene nuclei and a single carboxylic group; in addition the possible structures of four different R groupings are described in detail. The general process for the preparation of these compounds by reacting an amine with an acid chloride is given. Examples of the preparation of five specific compounds are also described, i.e. (1) 2,4,5-triiodo-3-hydroxymethyl-5-(2,4,6-triiodo-3-N-methylcarbamoyl-5-N-methyl-N-acetylamino-benzoyl)glycylamino-benzoic acid, (2) 2,4,6-triiodo-3-hydroxymethyl-5-(2,4,6-triiodo-3-N-methyl-N-acetylamino-benzoyl)glycylamino-benzoic acid, (3) 2,4,6-triiodo-3-hydroxymethyl-5-(2,4,6-triiodo-3-amino-5-N-methyl-N-acetylamino-benzoyl)glycylamino-benzoic acid, (4) 2,4,6-triiodo-3-hydroxymethyl-5-(2,4,6-triiodo-3-N-methylcarbamoyl-5-N-methyl-N-acetylamino-benzoyl)β-aminopropionyl-amino-benzoic acid and (5) 2,4,6-triiodo-3-hydroxymethyl-5-(2,4,6-triiodo-3-amino-5-N-methylcarbamoyl-benzoyl)glycyl-N-methylamino-benzoic acid. These X-ray contrast media are in the form of aqueous solutions of pharmaceutically acceptable salts. (UK)

  14. Simple Method To Detect β-Galactosidase

    OpenAIRE

    Bhowmik, Tarun; Marth, Elmer H.

    1989-01-01

    A simple and rapid method was developed to detect β-galactosidase by using α- or β-naphthyl-β-d-galactopyranoside as substrate and fast garnet GBC as a dye coupler following polyacrylamide gel electrophoresis. This method was specific for β-galactosidase but not for phospho-β-galactosidase.

  15. Biochemical study of resistance to imidacloprid in B-biotype Bemisia tabaci from Guatemala

    Science.gov (United States)

    Systemic uptake bioassays using excised cotton leaves confirmed resistance to imidacloprid in a Guatemalan population of the tobacco whitefly Bemisia tabaci Gennadius. Polyacrylamide gel electrophoresis of naphthyl esterases identified the insects as B-types. Upon collection from the field, resistan...

  16. Organometallic Methods for Forming and Cleaving Carbon-Carbon Bonds

    DEFF Research Database (Denmark)

    Christensen, Stig Holden

    lipophilic anchors and performing the dehydrogenative decarbonylation with the anchor monools proceeded well, while the corresponding anchor triols were unstable at the elevated temperatures. Of the simple primary alcohols investigated, 2-(2-naphthyl)ethanol, hexane-1,6-diol and dodecane-1,12-diol were found...

  17. Conformationally locked aryl C-nucleosides: synthesis of phosphoramidite monomers and incorporation into single-stranded DNA and LNA (locked nucleic acid)

    DEFF Research Database (Denmark)

    Babu, B. Ravindra; Prasad, Ashok K.; Trikha, Smriti;

    2002-01-01

    Synthesis of a series of LNA-type beta-configured C-aryl nucleosides, i.e., 2'- O,4'-C-methylene-beta-D-ribofuranosyl derivatives containing phenyl, 4-fluoro-3-methylphenyl, 1-naphthyl, 1-pyrenyl and 2,4,5-trimethylphenyl groups as aglycons, has been accomplished. The key synthetic step consisted...

  18. Solistatin, an aromatic compactin analogue from Penicillium solitum

    DEFF Research Database (Denmark)

    Sørensen, Dan; Larsen, Thomas Ostenfeld; Christophersen, Carsten; Nielsen, Per Halfdan; Anthoni, Uffe

    1999-01-01

    Solistatin, (+)-(3R,5R)-7-(2'-methyl-1'-naphthyl)-3-hydroxyheptan-5-olide (1), has been isolated from Penicillium solitum. The structure and relative stereochemistry were established by NMR spectroscopy and mass spectrometry. The absolute stereochemistry was determined by chemical degradation and...

  19. Improved Performance of Organic Light-Emitting Diodes with MgF2 as the Anode Buffer Layer

    Institute of Scientific and Technical Information of China (English)

    XIE Jing; ZHANG De-Qiang; WANG Li-Duo; DUAN Lian; QIAO Juan; QIU Yong

    2006-01-01

    @@ Organic light-emitting diodes (OLEDs) based on N,N'-bis(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4,4'-diamine (NPB) and tris (8-hydroxyquinoline) aluminium (Alq3) are improved by using a thin MgF2 buffer layer sandwiched between the indium tin oxide (ITO) anode and hole transporting layer (HTL) of NPB.

  20. Bimetallic lanthanide complexes that display a ratiometric response to oxygen concentrations

    OpenAIRE

    Sørensen, TJ; Kenwright, AM; Faulkner, S.

    2015-01-01

    A pair of hetero-bimetallic lanthanide complexes containing terbium and europium ions have been prepared by coupling kinetically stable complexes together using an Ugi methodology to incorporate a naphthyl chromophore. Both complexes exhibit emission from terbium and europium in solution. The terbium centred emission varies with dissolved oxygen concentration, while the europium intensity remains essentially constant in one of the complexes.

  1. 8-(Dimethylamino)naphthylcopper(I), a novel stable organocopper compound with unusual structural features. A study concerning its synthesis, structure (X-ray) and reactivity. Its synthesis, crystal structure (X-ray) and reactivity

    NARCIS (Netherlands)

    Koten, G. van; Wehman, E.; Knotter, M.; Spelten, H.; Heijdenrijk, D.; Mak, A.N.S.; Stam, C.H.

    1987-01-01

    The synthesis and isolation of a hydrocarbon- and ether-insoluble organocopper compound containing the rigid 8-(dimethylamino)naphthyl group is described. An X-ray determination of its structure revealed a tetranuclear copper aggregate, in which the Cu atoms are arranged in a parallelogram (Cu...Cu

  2. 4-[5-(2-Methoxyphenyl-1,3,4-oxadiazol-2-yl]benzohydrazide

    Directory of Open Access Journals (Sweden)

    Muhammad Taha

    2014-05-01

    Full Text Available 4-(5-(2-Methoxyphenyl-1,3,4-oxadiazol-2-ylbenzohydrazide (5 was synthesized by three steps. The synthesis started with 2-methoxybenzohydrazide to form hydrazone (3 which was then cyclized to oxadiazole (4 and finally, treatment of oxadiazole (4 with hydrazine hydrate afforded the final product (5.

  3. One-Step Synthesis of Sulfonamides from N-Tosylhydrazones.

    Science.gov (United States)

    Tsai, Andy S; Curto, John M; Rocke, Benjamin N; Dechert-Schmitt, Anne-Marie R; Ingle, Gajendrasingh K; Mascitti, Vincent

    2016-02-01

    The first described reaction between N-tosylhydrazone and SO2 is reported to provide alkyl sulfonamides in the presence of various amines. In this procedurally simple method, hydrazones of both unsaturated aldehydes and ketones proceed in moderate to excellent yields. Primary and secondary aliphatic amines are accommodated in this reaction, which provides a novel route to sulfonamides. PMID:26771228

  4. Investigation of adsorption of isoniazid derivatives at mild steel/hydrochloric acid interface: Electrochemical and weight loss methods

    International Nuclear Information System (INIS)

    The corrosion inhibition properties of isoniazid derivatives, namely N-(morpholino methyl) isatin-3-isonicotinoyl hydrazone (MIIH), N-(piperazino methyl) isatin-3-isonicotinoyl hydrazone (PIIH), N-(2-Thio benzimidazolyl methyl) isatin-3-isonicotinoyl hydrazone (TBIH), N-(piperadino methyl) isatin-3-isonicotinoyl hydrazone (PIIIH) for mild steel corrosion in 1 M HCl medium were analysed by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization and weight loss techniques. Electrochemical impedance data demonstrated that the addition of the isoniazid derivatives in the corrosive solution decreased the charge capacitance and simultaneously increased the function of the charge/discharge of the interface, facilitating the formation of an adsorbed layer over the steel surface. Adsorption of these inhibitors on the steel surface obeyed the Langmuir adsorption isotherm. Potentiodynamic polarization studies showed that all the tested inhibitors affected both the anodic and cathodic process, thus they can be classified as mixed type of inhibitor. The effect of chemical structure of the four tested inhibitors was discussed. It was found that the efficiency order followed by molecules tested was TBIH > PIIH > MIIH > PIIIH. Thus TBIH turned out to be the best inhibitor. This fact strongly suggests that, an efficient corrosion inhibitor molecule should be large one, planar, having unoccupied d-orbital and also containing an extensive number of π-electrons.

  5. Ruthenium complexes of salicylaldehyde benzoylhydrazones: synthesis and spectroscopic characterization

    International Nuclear Information System (INIS)

    Complex Ru(III) compounds with salicylidene hydrazones of benzoic and nicotinic acids are synthesized and investigated by the methods of element analysis, electron, NMR 1H and IR-spectroscopy and electrophoresis. It is shown that synthesis conditions effect on type of ligand coordination

  6. Polymer-doxorubicin conjugate with a synthetic peptide ligand targeted on prostate tumor

    Czech Academy of Sciences Publication Activity Database

    Pola, Robert; Pechar, Michal; Ulbrich, Karel; Fabra, A.

    2007-01-01

    Roč. 22, č. 6 (2007), s. 602-620. ISSN 0883-9115 R&D Projects: GA ČR GA204/05/2255 Institutional research plan: CEZ:AV0Z40500505 Keywords : drug delivery systems * drug research * hydrazones Subject RIV: CE - Biochemistry Impact factor: 1.917, year: 2007

  7. Coordination chemistry of actinide elements: preparation of new uranium complexes with schiff bases and their characterization (Preprint No. CT-31)

    International Nuclear Information System (INIS)

    The Schiff bases, o-vanillin semicarbazone (oVSC) and 2-pyridine carboxaldehyde isonicotinoyl hydrazone (PCINH) have been prepared and their novel complexes with dioxouranium(VI) have been synthesized and characterized by IR spectra, elemental analysis and other physico-chemical techniques. (author)

  8. HPMA copolymer-doxorubicin conjugates with pH-controlled activation

    Czech Academy of Sciences Publication Activity Database

    Etrych, Tomáš; Chytil, Petr; Mrkvan, Tomáš; Říhová, Blanka; Ulbrich, Karel

    Dresden : Max Planck Institute for the Physic of Complex Systems, 2005. [MPG-MOEL– Symposium: Science and Art in Europe, Polymers: Materials in Nature and in Advanced Technologies. 23.5.2005-25.5.2005, Dresden] R&D Projects: GA AV ČR(CZ) IAA4050201 Keywords : hydrazone * HPMA polymer * conjugates Subject RIV: CD - Macromolecular Chemistry

  9. Thieme Chemistry Journal Awardees - Where are They Now? Catalytic Transport with an Amine Carrier in a Fluorous Triphasic Reaction

    OpenAIRE

    Montanari, Vittorio; Yu, Marvin S.; Curran, Dennis P.

    2009-01-01

    Several aromatic aldehydes are transported by a fluorous amine from one organic phase through a fluorous phase to another organic phase. The derived imines react with phenylhydrazine to immobilize the transported product as a hydrazone and release the amine for reuse. In this way, catalytic transport is accomplished for the first time.

  10. Synthesis and Study of Novel Coumarin Derivatives Potentially Utilizable as Memory Media

    Directory of Open Access Journals (Sweden)

    Jana Donovalová

    2009-11-01

    Full Text Available Novel coumarin derivatives, 2-oxo-2H-chromenecarbaldehyde hydrazones were prepared by reaction of substituted 2-oxo-2H-chromenecarbaldehydes with N-aminoimides in ethanol in the presence of 4-toluenesulfonic acid as catalyst. The photochromic and thermochromic properties of the prepared compounds were investigated.

  11. Synthesis and Study of Novel Coumarin Derivatives Potentially Utilizable as Memory Media

    OpenAIRE

    Jana Donovalová; Anton Gáplovský; Radoslav Flašík; Henrieta Stankovičová

    2009-01-01

    Novel coumarin derivatives, 2-oxo-2H-chromenecarbaldehyde hydrazones were prepared by reaction of substituted 2-oxo-2H-chromenecarbaldehydes with N-aminoimides in ethanol in the presence of 4-toluenesulfonic acid as catalyst. The photochromic and thermochromic properties of the prepared compounds were investigated.

  12. Ultrasound-enhanced delivery of polymer-coated oncolytic adenovirus for tumour growth inhibition

    Czech Academy of Sciences Publication Activity Database

    Carlisle, R.; Choi, J.; Kostka, Libor; Bazan-Peregrino, M.; Ulbrich, Karel; Coussios, C.; Seymour, L.

    MARY ANN LIEBERT INC. Roč. 22, č. 10 (2011), A36. ISSN 1043-0342. [European Society of Gene and Cell Therapy British Society for Gene Therapy Collaborative Congress 2011. 27.10.2011-31.10.2011, Brighton] Institutional research plan: CEZ:AV0Z40500505 Keywords : coating * hydrazone bond Subject RIV: CD - Macromolecular Chemistry

  13. Synthesis, DNA-damaging and cytotoxic properties of novel topoisomerase II-directed bisantrene analogues.

    Science.gov (United States)

    Zagotto, G; Oliva, A; Guano, F; Menta, E; Capranico, G; Palumbo, M

    1998-01-20

    New bisantrene analogues were synthesized, bearing one or two 4,5-dihydro-1H-imidazol-2-yl hydrazone side chains at positions 1,4 or 9 of the anthracene ring system. A 10-azabioisostere was also prepared. The position of substituents in structurally isomeric drugs modulates topoisomerase II poisoning and specificity, along with cytotoxicity. PMID:9871638

  14. Injectable In Situ Forming Hybrid Iron Oxide-Hyaluronic Acid Hydrogel for Magnetic Resonance Imaging and Drug Delivery

    NARCIS (Netherlands)

    Zhang, Y; Sun, Y.; Yang, X.; Hilborn, J.; Heerschap, A.; Ossipov, D.A.

    2014-01-01

    The development of multimodal in situ cross-linkable hyaluronic acid nanogels hybridized with iron oxide nanoparticles is reported. Utilizing a chemoselective hydrazone coupling reaction, the nanogels are converted to a macroscopic hybrid hydrogel without any additional reagent. Hydrophobic cargos r

  15. A facile synthesis of novel bis-(indolyl)-1,3,4-oxadiazoles as potent cytotoxic agents.

    Science.gov (United States)

    Kumar, Dalip; Arun, V; Maruthi Kumar, N; Acosta, Glen; Noel, Brett; Shah, Kavita

    2012-11-01

    A recipe for potency: A novel series of bis(indolyl)-1,3,4-oxadiazoles was prepared from the corresponding hydrazide-hydrazones via iodobenzene diacetate-promoted oxidative cyclization. Evaluation against a panel of human cancer cell lines revealed that some derivatives possess potent cytotoxicity with tunable selectivity for different cancer types. PMID:22997171

  16. 1,3-Dipolar cycloadditions of ethoxycarbonyl-nitrile benzylimine and synthesis of ß-amino acids. Synthesis and reactions of ethyl 2-chloro-2-ethoxyacetate and 2-chloro-2-ethoxyacetylchloride

    DEFF Research Database (Denmark)

    Bach, K.K.; El-Seedi, H.R.; Jensen, H.M.; Nielsen, H.B.; Thomsen, I.; Torssell, K.B.G.

    1994-01-01

    -amines and subsequent hydrolysis gave beta-amino acids. The syntheses of the title reagents were described. Ethyl 2-chloro-2-ethoxy-acetate gave selectively oximes, hydrazones, nitrones, and phosphonium salts with hydroxylamine, hydrazines, N-substituted hydroxylamines and triphenylphosphine respectively...

  17. Combination topical therapy in the treatment of acne.

    Science.gov (United States)

    Del Rosso, James Q

    2006-08-01

    Many medications are available for the management of acne. The armamentarium includes topical retinoids (ie, adapalene, tazarotene, tretinoin), antimicrobial and antibacterial agents (ie, benzoyl peroxide, clindamycin, erythromycin, sulfacetamide with or without sulfur), oral antibiotics (ie, doxycycline, minocycline, tetracycline), hormonal agents (ie, oral contraceptives, spironolactone), and systemic retinoids (ie, isotretinoin). Acne usually is treated with combination therapy to address its multifactorial pathophysiology. The combination of clindamycin 1%-benzoyl peroxide 5% gel, available as a stable formulation in a single tube, is efficacious and well-tolerated. The product's excipients, glycerin and dimethicone, minimize treatment-related irritation, thereby increasing patient compliance. Clindamycin-benzoyl peroxide may be well-tolerated when applied with topical retinoids, creating a more targeted and complete treatment strategy. PMID:17966494

  18. 2-Chloro-N-(3-chlorophenylbenzamide

    Directory of Open Access Journals (Sweden)

    B. Thimme Gowda

    2008-07-01

    Full Text Available In the structure of the the title compound, C13H9Cl2NO, the N—H and C=O groups are mutually trans. Furthermore, the conformation of the C=O group is syn to the ortho-chloro group in the benzoyl ring, while the N—H bond is anti to the meta-chloro group in the aniline ring. The amide group forms dihedral angles of 89.11 (19 and 22.58 (37°, respectively, with the benzoyl and aniline rings, while the benzoyl and aniline rings form a dihedral angle of 69.74 (14°. The molecules are linked into infinite chains through intermolecular N—H...O hydrogen bonds.

  19. Synthesis and antitumor activity of 2-. beta. -D-ribofuranosylselenazole-4-carboxamide and related derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Srivastava, P.C.; Robins, R.K.

    1983-01-01

    Treatment of 2,3,5-tri-O-benzoyl-..beta..-D-ribofuranosyl-1-carbonitrile with hydrogen selenide provided 2,5-anhydro-3,4,6-tri-O-benzoyl-D-allonselenoamide (3). Compound 3 was treated with ethyl bromopyruvate to provide ethyl 2-(2,3,5-tri-O-benzoyl-D-ribofuranosyl)selenazole-4-carboxylates, which after ammonolysis were converted to 2-..beta..-D-ribofuranosylselenazole-4-carboxamide (6) and its ..cap alpha..-analogue 7, respectively. Acetylation of nucleoside 6 provided 2-(2,3,5-tri-O-acetyl-..beta..-D-ribofuranosyl)selenazole-4-carboxamide, and phosphorylation of 6 provided the corresponding 5'-phosphate 9. Compounds 6 and 9 were found to be cytotoxic toward P388 and L1210 cells in culture and effective against Lewis lung carcinoma in mice.

  20. N-(4-Chlorophenyl-2-methylbenzamide

    Directory of Open Access Journals (Sweden)

    Hartmut Fuess

    2009-02-01

    Full Text Available In the structure of the title compound, C14H12ClNO, the N—H and C=O bonds are trans to each other. Furthermore, the C=O bond is syn to the ortho-methyl group in the benzoyl ring, similar to what is observed in 2-methyl-N-(4-methylphenylbenzamide and 2-methyl-N-phenylbenzamide. The amide linkage (–NHCO– makes dihedral angles of 36.9 (7 and 46.4 (5° with the aniline and benzoyl rings, respectively, while the dihedral angle between the benzoyl and aniline rings is 83.1 (1°. In the crystal structure, molecules form chains running along the b axis through N—H...O hydrogen bonds.

  1. N-(2-Chlorophenyl-2-methylbenzamide

    Directory of Open Access Journals (Sweden)

    B. Thimme Gowda

    2008-08-01

    Full Text Available In the structure of the title compound (N2CP2MBA, C14H12ClNO, the conformations of the N—H and C=O bonds are trans to each other. Furthermore, the conformation of the N—H bond is syn to the ortho-chloro group in the aniline ring and the C=O bond is syn to the ortho-methyl substituent in the benzoyl ring, similar to what is observed in 2-chloro-N-(2-chlorophenylbenzamide and 2-methyl-N-phenylbenzamide. The amide group makes almost the same dihedral angles of 41.2 (14 and 42.2 (13° with the aniline and benzoyl rings, respectively, while the dihedral angle between the benzoyl and aniline rings is only 7.4 (3°. The molecules in N2CP2MBA are packed into chains through N—H...O hydrogen bonds.

  2. Limonoids of the phragmalin type from Swietenia macrophylla and their chemotaxonomic significance.

    Science.gov (United States)

    da Silva, Milton Nascimento; Arruda, Mara Silvia Pinheiro; Castro, Kelly Christina F; da Silva, M Fátima das G F; Fernandes, João B; Vieira, Paulo C

    2008-12-01

    Species of Swietenia elaborate limonoid chemistry along only one route, which leads to the mexicanolide type in most species and the phragmalin type in S. mahogani. A hexane extract from leaves of S. macrophylla afforded six new phragmalins with a 8,9,30-ortho-ester unit, namely, 6-O-acetylswietephragmin E (1), 3beta-O-destigloyl-3beta-O-benzoyl-6-O-acetylswietephragmin E (2), 12alpha-acetoxyswietephragmin C (3), 3beta-O-destigloyl-3beta-O-benzoyl-12alpha-acetoxyswietephragmin C (4), 12alpha-acetoxyswietephragmin D (5), and 3beta-O-destigloyl-3beta-O-benzoyl-12alpha-acetoxyswietephragmin D (6). This appears to be the first record of phragamalins from S. macrophylla, and this study shows the potential of tricyclic [3.3.1(2,10).1(1,4)]-decane limonoids as taxonomically useful chemical markers in the Meliaceae. PMID:19053509

  3. Chemical Constituents from Stem Bark and Roots of Clausena anisata

    Directory of Open Access Journals (Sweden)

    Etienne Dongo

    2012-11-01

    Full Text Available Phytochemical investigations on the stem bark and roots of the tropical shrub Clausena anisata led to the isolation and characterization three carbazole alkaloids: girinimbine, murrayamine-A and ekeberginine; two peptide derivatives: aurantiamide acetate and N-benzoyl-l-phenylalaninyl-N-benzoyl-l-phenylalaninate; and a mixture of two phytosterols: sitosterol and stigmasterol. The structures of these compounds were established by nuclear magnetic resonance (1H-NMR, 13C-NMR, COSY, HSQC, HMQC, HMBC and NOESY spectroscopy and electrospray ionization mass spectrometry (MS.

  4. (4bS,8aS-1-Isopropyl-4b,8,8-trimethyl-4b,5,6,7,8,8a,9,10-octahydrophenanthren-2-yl benzoate

    Directory of Open Access Journals (Sweden)

    Radouane Oubabi

    2014-08-01

    Full Text Available The title compound, C27H34O2, was hemisynthesized through direct benzoylation of the naturally occurring meroterpene totarol. The central fused six-membered ring has a half-chair conformation, whereas the terminal six-membered ring displays a chair conformation. The dihedral angle between the fused benzene ring and the benzoyl benzene ring is 73.05 (14°. The S,S chirality of the molecule is consistent with the synthetic pathway, and confirmed by the refinement of the Flack parameter.

  5. X-ray diffraction analysis and study of thermal stability of benzo acetonates of some transition group metals

    International Nuclear Information System (INIS)

    Crystals of benzoyl acetonates of Mn (II), Cd (II) and Fe (III) have been prepared. Their structures have been determined by X-ray powder diffraction. Thermogravimetric analysis (TGA) of these benzoyl acetonate indicate that they are stable up to 90 deg. C,220 deg. C, 65 deg. C, and 190 deg. C respectively. It is found that the thermal stability of the transition meals chelates follows the order Cd/sup 2+/ < Mn/sup 2+/ < Fe/sup 3+/< Ni/sup 2+/. The chelate of Cd(II) (last member of the second transition series) has the lowest temperature of decomposition of all the compounds studied. (author)

  6. A Novel Approach to the Synthesis of 6-Amino-7-hydroxy-flavone

    Directory of Open Access Journals (Sweden)

    Tianyu Zhuang

    2004-09-01

    Full Text Available A novel approach to the synthesis of 6-amino-7-hydroxyflavone (1 is described. Reaction in acetone of 2′,4′-dihydroxy-5′-nitroacetophenone and benzoyl chloride in the presence of potassium carbonate affords 3-benzoyl-7-hydroxy-6-nitroflavone, which is cleaved in 5% ethanolic potassium hydroxide to give 1-(2,4-dihydroxy-5-nitrophenyl-3- phenyl-1,3-propanedione. The 1,3-diketone thus formed is then transformed into 7-hydroxy- 6-nitroflavone, followed by reduction to afford the title compound.

  7. Coexistence of spin-crossover and magnetic ordering in the dendrimeric Fe(III) complex

    International Nuclear Information System (INIS)

    The magnetic properties of the dendrimeric spin-crossover Fe(III) complex of formula [Fe(L)2]+PF6-, where L = 3,5-di[3,4,5-tris(tetradecyloxy) benzoyl-oxy]benzoyl-4-salicylidene-N'-ethyl-N-ethylene-diamine are reported for the first time. EPR spectroscopy shows that the compound displays a gradual spin-crossover in the temperature range (70-300 K) and undergoes an antiferromagnetic ordering below 10 K. Mossbauer spectroscopy data confirm the existence of magnetic ordering at 5 K in the Fe(III) dendrimeric complex.

  8. Palladium-catalyzed N-acylation of monosubstituted ureas using near-stoichiometric carbon monoxide.

    Science.gov (United States)

    Bjerglund, Klaus; Lindhardt, Anders T; Skrydstrup, Troels

    2012-04-20

    The palladium-catalyzed carbonylation of urea derivatives with aryl iodides and bromides afforded N-benzoyl ureas (20 examples) in yields attaining quantitative via the application of near-stoichiometric amounts of carbon monoxide generated from the decarbonylation of the CO precursor, 9-methylfluorene-9-carbonyl chloride. The synthetic protocol displayed good functional group tolerance. The methodology is also highly suitable for (13)C isotope labeling, which was demonstrated through the synthesis of three benzoyl ureas, including the insecticide triflumuron, whereby (13)CO was incorporated into the core structure. PMID:22458554

  9. N-(4-Chlorophenylbenzamide

    Directory of Open Access Journals (Sweden)

    Hartmut Fuess

    2008-04-01

    Full Text Available The structure of the title compound, C13H10ClNO, resembles those of N-phenylbenzamide, N-(2-chlorophenylbenzamide and other benzanilides, with similar bond parameters. The amide group –NHCO– makes a dihedral angle of 29.95 (9° with the benzoyl ring, while the benzoyl and aniline rings form a dihedral angle of 60.76 (3°. The structure shows both intra- and intermolecular hydrogen bonding. The molecules are linked by N—H...O hydrogen bonds into chains running along the [100] direction.

  10. Synthesis, characterization, crystal structures, and antibacterial activity of some new 1-(3,4,5-trimethoxybenzoyl)-3-aryl thioureasreas

    OpenAIRE

    Saeed, Aamer; Khera, Rasheed Ahmad; Abbas, Naeem; Latif, Muhammad

    2010-01-01

    Synthesis of some novel 1-(3,4,5-trimethoxy)benzoyl-3- arylthiourea derivatives (1a-o) was accomplished in 2 steps. The synthetic route involves the reaction of 1-(3,4,5-trimethoxy)benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in acetone to afford the corresponding isothiocyante followed by treatment with suitably substituted anilines. The structures of the products were established by elemental analyses, IR, 1H- and 13C-NMR, and mass spectroscopy and for 1b and 1m f...

  11. Studies in Multifunctional Drug Development: Preparation and Evaluation of 11beta-Substituted Estradiol-Drug Conjugates, Cell Membrane Targeting Imaging Agents, and Target Multifunctional Nanoparticles

    Science.gov (United States)

    Dao, KinhLuan Lenny D.

    with an azido-tetraethylene glycol moiety that could be coupled to a complementary doxorubicin benzoyl hydrazone, functionalized with a propargyl tetraethylene glycol moiety. Huisgen [3+2] cycloaddition chemistry gave the final hybrid which was evaluated for receptor binding to demonstrate ER-affinity and for cytotoxicity in ER(+)-MCF-7 and ER(-)-MDA-MB-231 breast cancer cell lines. The anti-estrogen-doxorubicin hybrid demonstrated enhanced (>70-fold) selectivity for ER(+)-cells versus ER(-)-cells and enhanced efficacy compared to doxorubicin alone. The reversal of these effects by co-administration of estradiol demonstrated that the presence of the anti-estrogenic component was critical for selectivity and cytotoxicity in ER(+)-MCF-7 human breast cancer cells. The results suggest that this approach the basis for developing selective therapeutic agents for ER(+)-cancer cells with reduced effects on non-target tissues.1,2 The second study describes our use of 11beta-AE for targeting ER membrane targeting in hormone-dependent breast cancer, and of a urea-based prostate specific membrane antigen (PSMA) inhibitor for targeting PSMA membrane receptors in androgen-independent of prostate cancer. These derivatives were used to prepare a series of molecular imaging probes. We have successfully established our model compound, 11beta-AE radiolabeled with 18F-fluoro-OEG-azide, for in vivo imaging.3 The third study describes a strategy based on the design and synthesis of a multifunctional gold nanoparticulate (mfAuNPs) drug delivery system that can be used for prostate cancer therapy. We have utilized a convergent modular assembly approach to prepare individual components such as a) prostate specific membrane antigen (PSMA) ligands for targeting; b) pH-sensitive doxorubicin; and c) Re/99Tc chelating complex for radioimaging. The components can be assembled with a terminal lipoic acid or thiolated ethylene glycol oligomer for attachment to the Au surface. Initial in vitro studies

  12. New Developments in Acne Treatment

    OpenAIRE

    Stolman, Lewis P.

    1982-01-01

    Acne is a metabolic disorder of the pilosebaceous appendage in which microorganisms, hormones, inflammatory cells and fatty acids seem to contribute to the pathologic process. Through education and judicious use of therapeutic agents including benzoyl peroxide, vitamin A acid, topical and systemic antibiotics and 13 cis retinoic acid, most patients with acne can enjoy good control of their disease.

  13. Grafted Cross-Linked Polyolefin Substrates for Peptide Synthesis and Assays

    DEFF Research Database (Denmark)

    1999-01-01

    organic peroxide such as benzoyl peroxide, to which substrate are grafted polymer chains such as polystyrene chains which are functionalized with a chemical functionality facilitating the formation of an anchoring linkage between the polymer moiety and another chemical species. The solid support is also...

  14. Influence of Bleaching on Flavor of 34% Whey Protein Concentrate and Residual Benzoic Acid Concentration in Dried Whey Proteins

    Science.gov (United States)

    Previous studies have shown that bleaching negatively affects the flavor of 70% whey protein concentrate (WPC70), but bleaching effects on lower-protein products have not been established. Benzoyl peroxide (BP), a whey bleaching agent, degrades to benzoic acid (BA) and may elevate BA concentrations...

  15. PTSA CATALYZED KSF SOLID SUPPORTED MICHAEL ADDITION ON STYRYLISOXAZOLES AND THEIR REDUCTIVE CYCLIZATION TO AZEPINES PTSA KATALYSIERTEN KSF SOLID UNTERSTÜTZTE MICHAEL zusätzlich auf STYRYLISOXAZOLES UND IHRE reduktive Cyclisierung zu Azepinen

    Directory of Open Access Journals (Sweden)

    E. Rajanarendar, P. Ramesh, Firoz Pasha Shaik , M. Srinivas

    2011-04-01

    Full Text Available The Michel addition of styrylisoxazoles with ethyl benzoyl acetate in presence of ptoluene sulfonic acid (PTSA catalyst supported on KSF solid furnished the Michael adducts in excellent yields in short time. The Michael adducts underwent reductive cyclization on treatment with SnCl2- MeOH to afford isoxazolo [4,5-b] azepines in high yields.

  16. Redox Polymerization of Methyl Methacrylate in the Fluorous Triphasic System

    Institute of Scientific and Technical Information of China (English)

    Shi Zhen CHEN; Yun Peng BAI; Zhao Long LI

    2006-01-01

    Methyl methacrylate (MMA) was polymerized by using of benzoyl peroxide (BPO) and N, N-dimethylaniline (DMA) as an redox initiator in fluorous triphasic system at room temperature.The polymerization was occurred in both initiator layer and monomer layer in a U-tube. It was found that PMMA obtained from the initiator layer with relatively narrow polydispersity.(PDI =1.38)

  17. Synthesis and infrared and moessbauer spectrometric study of europium(3) complexes with some derivatives of semi- and thiosemicarbazide

    International Nuclear Information System (INIS)

    Europium complexes with semi- and thiosemicarbazidediacetic acid, as well as thiosemicarbazones of glyoxylic, pyruvic and benzoyl formic acids have been investigated by the methods of infrared and the Moessbauer spectroscopy. It is established that the resonance absorption effect constitutes a value of one order and testifies to their polymeric structure

  18. Synthesis of acrylic prepolymer

    International Nuclear Information System (INIS)

    An acrylic prepolymer was synthesized from glycidyl methacrylate (GMA), butyl methacrylate (BMA), methyl methacrylate (MMA) and acrylic acid (AA). Butyl acetate (BAc), benzoyl peroxide (BzO), 4-methoxyphenol (MPh) and triethylamine (TEA) were used as solvent, initiator, inhibitor and catalyst respectively. Observations of the synthesis leading to the formation of acrylic prepolymer are described. (author)

  19. Studies on the Structure of Kansuinine A from Euphorbia kansui

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Kansuinine A is a macrocyclic jatrophane diterpene that was isolated from Euphorbia kansui. Further investigation of the structure was revealed that the benzoyl group located at C-8 and the position of C-3 was the present of an acetyl group by means of HMQC, HMBC spectra.

  20. 2-(4-Diethoxymethylphenyl-6-(4-nitrophenyl-4-phenyl-1,3-diazabicyclo[3.1.0]hex-3-ene

    Directory of Open Access Journals (Sweden)

    Hamzeh Kiyani

    2012-09-01

    Full Text Available The photochromic compound was obtained from 4-diethoxymethyl-benzaldehyde and trans-2-benzoyl-3-(4-nitrophenylaziridine via a three component reaction. The structure of this compound was characterized by elemental analysis, 1H-NMR, 13C-NMR and UV-Visible spectral data.

  1. Hydrocyanation of sulfonylimines using potassium hexacyanoferrate(II) as an eco-friendly cyanide source

    Energy Technology Data Exchange (ETDEWEB)

    Li, Zheng; Li, Rongzhi; Zheng, Huanhuan; Wen, Fei; Li, Hongbo; Yin, Junjun; Yang, Jingya, E-mail: lizheng@nwnu.edu.cn [Key Laboratory of Eco-Environment-Related Polymer Materials for Ministry of Education, College of Chemistry and Chemical Engineering, Northwest Normal University, Gansu (China)

    2013-11-15

    An efficient and eco-friendly method for hydrocyanation of sulfonylimines via one-pot two-step procedure using potassium hexacyanoferrate)II) as cyanide source, benzoyl chloride as a promoter, and potassium carbonate as a base is described. This protocol has the features of using nontoxic, nonvolatile and inexpensive cyanide source, high yield, and simple work-up procedure. (author)

  2. Synthesis of carbon-14 labeled doxylamine succinate

    International Nuclear Information System (INIS)

    Doxylamine succinate, N,N-dimethyl-2-[1-phenyl-1-(2-pyridinyl)-ethoxy]ethanamine succinate is an antihistamine used primarily as a sedative. Carbon-14 labeled doxylamine succinate, required for toxicological studies, was synthesized in two steps starting from 2-benzoyl pyridine. (author)

  3. Unedoside derivatives in Nuxia and their biosynthesis

    DEFF Research Database (Denmark)

    Jensen, Søren Rosendal; Ravnkilde, Lene; Schripsema, Jan

    1998-01-01

    isolated, while from N. oppositifolia 2 "-acetyl-3 "-benzoyl-nuxioside was obtained. Both plants contained verbascoside. The biosynthesis of unedoside in N. floribunda was investigated and deoxyloganic acid was found to be a precursor, similar to wh;lt was found for the eight-carbon iridoids in Thunbergia...

  4. Chemotaxonomy of the genus Nuxia (Buddlejaceae)

    DEFF Research Database (Denmark)

    Jensen, Søren Rosendal

    1999-01-01

    ''-cinnamoyl-nuxioside, while from N. oppositifolia was obtained 2''-acetyl-3''-benzoyl-nuxioside. Verbascoside was isolated from both plants. The biosynthesis of unedoside in N. floribunda was investigated and deoxyloganic acid was shown to be a precursor. The taxonomic position of Nuxia and Buddlejaceae is...

  5. Preparation of polystyrene-poly(ethylene glycol) diblock copolymer by "living" free radical polymerization

    DEFF Research Database (Denmark)

    Chen, Xianyi; Gao, Bo; Kops, Jørgen;

    1998-01-01

    Amphiphilic diblock copolymer containing segments of polystyrene and monomethoxypoly(ethylene glycol) (PS-b-PEG) was synthesised by a novel method. Initially, the adduct (BZ-TEMPO) obtained by reacting benzoyl peroxide, styrene, and 2,2,6,6-tetramethyl-piperidinyl-1-oxy (TEMPO) was isolated...

  6. Use of Cyclic Di- and Triperoxides as Initiators of Styrene Polymerization at High Temperature with a View to Their Use in Industrial Applications

    OpenAIRE

    A. I. Cañizo; Cerna, J. R.; Eyler, G. N.; Morales, G.

    2000-01-01

    In industry, the bulk free radical polymerization of styrene takes place with the aid of peroxide initiators such as benzoyl peroxide. In this work di- and trimeric cyclic peroxides were used as initiators of the styrene polymerization in order to increase the rate of polymerization and molecular weights simultaneously.

  7. Safe Preparation of HCl and DCl for IR Spectroscopy

    Science.gov (United States)

    Furlong, William R.; Grubbs, W. Tandy

    2005-01-01

    The widely used method of synthesizing HCl and DCl gases for infrared analysis by hydrolysis of benzoyl chloride includes a potentially dangerous final step whereby the frozen product is allowed to heat and expand into an infrared gas cell. The subsequent rapid rise in vapor pressure can "pop" open glass joints in the vacuum line and vent the…

  8. Disciplined Reactions - A Facile One-Flask Synthesis of 2-Substituted-4-m-methoxy -p-hydroxybezylidene-1-phenyl-2-imidazolin-5-ones and its Biological Evaluation.

    Directory of Open Access Journals (Sweden)

    Aditi Taunk

    2013-08-01

    Full Text Available Condensation reactions of N-acetyl-, N-benzoyl and N-ptolylglycines with vanillin in presence of isothiocyanate gives 2-m-methoxyp- hydroxystyryl-, 2-p-tolyl- and 2-phenyl -4-m-methoxy- phydroxybenzylidene- 1-phenyl-2-imidazolin-5-ones respectively. These compounds were evaluated in vitro for antibacterial activity.

  9. Drug: D03093 [KEGG MEDICUS

    Lifescience Database Archive (English)

    Full Text Available D03093 Drug Benzoyl peroxide (JAN/USP) C14H10O4 242.0579 242.2268 D03093.gif Keratolytic Same as ... sification [BR:br08303] D DERMATOLOGICALS D10 ANTI-ACNE ... PREPARATIONS D10A ANTI-ACNE ... PREPARATIONS FOR TOPIC ...

  10. The "Mushroom Cloud" Demonstration Revisited

    Science.gov (United States)

    Panzarasa, Guido; Sparnacci, Katia

    2013-01-01

    A revisitation of the classical "mushroom cloud" demonstration is described. Instead of aniline and benzoyl peroxide, the proposed reaction involves household chemicals such as alpha-pinene (turpentine oil) and trichloroisocyanuric acid ("Trichlor") giving an impressive demonstration of oxidation and combustion reactions that…

  11. 3-tert-Butyl-4-oxo-3,4-dihydro­phthalazin-1-yl 3,5-dimethyl­benzoate

    OpenAIRE

    Dao-Xin Wu; Zheng-Wang Chen; Ye-Guo Ren; Ming-Zhi Huang

    2007-01-01

    The title compound, C21H22N2O3, was synthesized by the reaction of tert-butylhydrazine with phthalic anhydride and further O-benzoylation of the resulting intermediate by 3,5-dimethylbenzoyl chloride. Intermolecular C—H...O=C interactions link the molecules into layers.

  12. 3-tert-Butyl-4-oxo-3,4-dihydrophthalazin-1-yl 3,5-dimethylbenzoate

    Directory of Open Access Journals (Sweden)

    Dao-Xin Wu

    2008-01-01

    Full Text Available The title compound, C21H22N2O3, was synthesized by the reaction of tert-butylhydrazine with phthalic anhydride and further O-benzoylation of the resulting intermediate by 3,5-dimethylbenzoyl chloride. Intermolecular C—H...O=C interactions link the molecules into layers.

  13. Gclust Server: 12219 [Gclust Server

    Lifescience Database Archive (English)

    Full Text Available 12219 Rpa1_RPE_0608 Cluster Sequences - 394 benzoyl-CoA reductase, subunit C 9 1.00...e-16 0.0 0.0 0.0 26.67 9.68 0.0 Show 12219 Cluster ID 12219 Sequence ID Rpa1_RPE_0608 Link to cluster sequen

  14. 21 CFR 133.102 - Asiago fresh and asiago soft cheese.

    Science.gov (United States)

    2010-04-01

    ... fat therefrom or by adding thereto one or more of the following: Cream, skim milk, concentrated skim... weight of the benzoyl peroxide used. If milk is bleached in this manner, sufficient vitamin A is added to the curd to compensate for the vitamin A or its precursors destroyed in the bleaching process,...

  15. 21 CFR 133.165 - Parmesan and reggiano cheese.

    Science.gov (United States)

    2010-04-01

    ... or by adding thereto one or more of the following: Cream, skim milk, concentrated skim milk, nonfat... weight of the benzoyl peroxide used. If milk is bleached in this manner, sufficient vitamin A is added to the curd to compensate for the vitamin A or its precursors destroyed in the bleaching process,...

  16. Oxidative Debenzylation and Acetylation of Hexabenzylhexaazaisowutzitane

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The oxidative reactivity of hexabenzylhexaazaisowutzitane(HBIW)under different conditions was studied. It was found that the N-benzyl groups were found to form benzoyl group after oxidation. They might also be first debenzylated and then acetylated by potassium permanganate in acetic anhydride/DMF.

  17. Coordination compounds of manganese(2) and cadmium(2) with α-ketoacid thiosemicarbazones

    International Nuclear Information System (INIS)

    Manganese (2) and cadmium (2) coordination compounds with gluoxalic, pyroacemic and benzoyl formic acid thiosemicarbazones are synthesized. ESR spectra of polycrystalline samples of manganese compounds and cadmium compounds activated with manganese at T=113 295 deg K allow to suppose that Mn2+ takes the position of Cd2+ ion which is in a weakly distorted octahedron crystal field

  18. 1,4-Bis{(+-(S-[1-(1-naphthylethyl]iminomethyl}benzene

    Directory of Open Access Journals (Sweden)

    Armando Espinosa Leija

    2009-10-01

    Full Text Available The title compound, C32H28N2, is a chiral bis-imine in which both imine groups display the common E configuration. The naphthyl groups present different orientations with respect to the central core, as reflected in the dihedral angles of 21.4 (2 and 78.83 (14° between the benzene and naphthyl mean planes, thus the highest possible C2 local molecular symmetry is not attained. This C1 molecular conformation allows multiple C—H...π intermolecular contacts involving all aromatic rings, while no π–π interactions are available for the stabilization of the crystal structure. The resulting packing structure is based on molecules stacked along [100].

  19. Localized operator partitioning method for electronic excitation energies in the time-dependent density functional formalism

    CERN Document Server

    Nagesh, Jayashree; Brumer, Paul; Izmaylov, Artur F

    2016-01-01

    We extend the localized operator partitioning method (LOPM) [J. Nagesh, A.F. Izmaylov, and P. Brumer, J. Chem. Phys. 142, 084114 (2015)] to the time-dependent density functional theory (TD-DFT) framework to partition molecular electronic energies of excited states in a rigorous manner. A molecular fragment is defined as a collection of atoms using Stratman-Scuseria-Frisch atomic partitioning. A numerically efficient scheme for evaluating the fragment excitation energy is derived employing a resolution of the identity to preserve standard one- and two-electron integrals in the final expressions. The utility of this partitioning approach is demonstrated by examining several excited states of two bichromophoric compounds: 9-((1-naphthyl)-methyl)-anthracene and 4-((2-naphthyl)-methyl)-benzaldehyde. The LOPM is found to provide nontrivial insights into the nature of electronic energy localization that are not accessible using simple density difference analysis.

  20. An aromatic region to induce a switch between agonism and inverse agonism at the ghrelin receptor

    DEFF Research Database (Denmark)

    Els, Sylvia; Schild, Enrico; Petersen, Pia Steen;

    2012-01-01

    The ghrelin receptor displays a high constitutive activity suggested to be involved in the regulation of appetite and food intake. Here, we have created peptides with small changes in the core binding motif -wFw- of the hexapeptide KwFwLL-NH(2) that can swap the peptide behavior from inverse......-tryptophane at position 4 with 1-naphthyl-d-alanine (d-1-Nal) and 2-naphthyl-d-alanine (d-2-Nal) induces agonism in functional assays. Competitive binding studies showed a high affinity of the inverse agonist K-(d-1-Nal)-FwLL-NH(2) at the ghrelin receptor. Moreover, mutagenesis studies of the receptor revealed key...