• Title/Summary/Keyword: o-Phenylenediamine

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Synthesis, Characterization and Catalytic Application of MoO3/CeO2-ZrO2 Solid Heterogeneous Catalyst for the Synthesis of Benzimidazole Derivatives

  • Rathod, Sandip B.;Lande, Machhindra K.;Arbad, Balasaheb R.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2835-2840
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    • 2010
  • A series of $MoO_3/CeO_2-ZrO_2$ catalysts with different Mo content (8 - 20 wt %) were prepared by simple co-precipitation followed by impregnation method and were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), energy dispersive spectroscopic (EDS) techniques. The prepared materials were tested for catalytic activity by the synthesis of benzimidazole derivatives using condensation of aromatic aldehydes and o-phenylenediamine by conventional and microwave method. Obtained results reveal that the catalytic activity increases with increase in Mo wt % loading. The best catalytic activity was obtained with 20 wt % $MoO_3/CeO_2-ZrO_2$. The particle size or crystallite size was estimated using Debye-Scherrer equation. After completion of reaction, the catalyst can be recovered efficiently and reused with consistent activity.

Synthesis of Several New Isoxazole, Imidazo[1, 2-a]pyridine, Imidazo[1, 2-a]pyrimidine, Benzoxadiazine and Benzothiazine Derivatives from Hydroximoyl Halides

  • Abdelhamid, Abdou O.;Abdou, Sadek E.;Mahgoub, Sayed A.
    • Archives of Pharmacal Research
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    • v.15 no.4
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    • pp.317-321
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    • 1992
  • Furoyldroximoyl chloride 3d reacted with 2-aminopyridine, 2-aminopyrimidine. O-aminophenol, O-phenylenediamine and aminothiophenol to afford imidazo [1, 2-a]pyridine 6. imidazo[1, 2-a]pyrimidine 8, benzoxadiazine 10, nitrosobenzopyrizine 13a and nitrosobenzothiazine 13b, respectively. Isoxazoline 18 and pyrrolidino[3, 4-d]isoxazolin-4, 6-dione derivatives 19a and 19b obtained by the reaction of 3 with acrylonitrile and N-arylmaleimide. Hydroximoyl chloride 3 reacted with thiophenol and sodium benzene-sulfinate to yield furylglyoxaloxime 16a and 16b, respectively. Hydroximoyl chloride 3 reacted also with some active methylene compound to give isoxazole derivatives 20-23, respectively.

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Studies on the Development of Iodine Recovery Process with High Yield and Purity from NH4I Solution (NH4I 용액으로부터 고효율/고순도의 요오드 회수 공정개발에 관한 연구)

  • Yoon, Jong Sun;Lim, Seong Bin;Oh, Se Yong
    • Applied Chemistry for Engineering
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    • v.26 no.3
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    • pp.377-380
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    • 2015
  • In this paper, we have investigated the optimization of $I_2$ recovery process from $NH_4I$ solution, which is generated as by-product during the amination reaction of p-diiodobenzene (PDIB) for p-phenylenediamine (PPD) synthesis. The recovered $I_2$ is then recycled as a raw material for PDIB synthesis. We have employed a cation exchange resin to recover $I_2$ from $NH_4I$ sample solution, and determined the breakthrough point and exchange capacity from the breakthrough curve. Furthermore, we have suggested optimum conditions of our $I_2$ recovery process by measuring the purity and yield of recovered $I_2$ with respect to the concentrations of $NH_4I$ and oxidant ($H_2O_2$) solutions, the oxidation time, and the temperature of drying process. Finally, the yield and purity as high as 94.96% and 96.65%, respectively were obtained by reusing the residual solution still containing unrecovered iodide ions.

Inactivation of Peroxidase from Fuji Apples by Heat and Chemical Treatments (가열 및 화합물에 의한 후지 사과 Peroxidase의 활성억제)

  • Choi, Eon-Ho;Jung, Dong-Sun
    • Applied Biological Chemistry
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    • v.30 no.3
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    • pp.285-290
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    • 1987
  • As a basic research for inhibition of enzymatic browning of apples during dehydration or processing, peroxidase was extracted from Fuji apples to investigate heat inactivation, and chemical inhibition. Peroxidase showed the highest activity at $35^{\circ}C$ and pH 5.5 using substrates of p-phenylenediamine and $H_2O_2$. The thermal inactivation followed biphasic kinetics to have activation energy (Ea) of 48.2kcal/mol and z value of $11.2^{\circ}C$ for the heat labile fraction and Ea of 36.3kcal/mol and z value of $14.9^{\circ}C$ for the heat resistant fraction. Browning by peroxidase was completely inhibited at the concentrations of 10mM for sodium diethyldithiocarbamate and potassium metabisulfite and 1mM for L-cysteine and ascorbic acid.

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Metal-Nitrosyl Complexes (I) Synthesis and Characterization of Dinitrosylmolybdenum (O) Complexes (금속-니트로실 착물 (제 1 보) 디니트로실몰리브덴(O) 착물의 합성과 특성)

  • Oh Sang-Oh;Mo Seong-Jong
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.661-668
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    • 1992
  • The polymeric compound [{Mo(NO)_2Cl_2}n] was prepared by reductive nitrosylation of NaNO_2 and acidified FeSO_4 with MoCl_5. The reactions of [{Mo(NO)_2Cl_2}n] with unidentate and bidentate ligands afforded neutral monomeric $[Mo(NO)_2Cl_2L_2(or L-L)] in high yield (80∼90%). 3,5-Lutidine, {\gamma}-Cyanopyridine, 1,2-Phenylenediamine, 1,10-Phenanthroline, sym-Diphenylethylenediamine, 9,10-Phenanthrenequinone, 1,3-Bis(diphenylphosphino)propane and 8-Hydroxyquinoline were used as coordinating ligands. The preparation and characterization of these dinitrosylmolybdenum complexes by elemental analysis, 1H NMR, infrared, and UV-Visible spectroscopy are reported. The infrared spectra indicate that in all of the compounds prepared, the NO groups occupy cis-positions in the octahedral group of ligands.

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Metal-Nitrosyl Complexes(II) : Synthesis and Characterization of Dinitrosyltungsten(O) Complexes (금속-니트로실 착물 (제 2 보) : 디니트로실 텅스텐(O) 착물의 합성과 특성)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • v.36 no.6
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    • pp.906-913
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    • 1992
  • The polymeric compound [{$W(NO)_2Cl_2$}$_n$] were prepared by reductive nitrosylation of $WNaNO_2$ and acidified $WFeSO_4$ with $WWCl_6$ at room temperature. The reactions of [{$W(NO)_2Cl_2$}$_n$] with unidentate and bidentate ligands afforded neutral monomeric [$W(NO)_2Cl_2L_2$(or L-L)] in a relative high yields (70$\sim$90%). 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene and 8-hydroxyquinoline were used as coordinating ligands. These dinitrosyltungsten complexes were characterized by elemental analysis, $^1H$-NMR, infrared, and UV-visible spectroscopy are reported. The spectral data indicated that geometric structures of the products were cis-dinitrosyl-trans-dichloro-cis-$L_2$ of $C_{2v}$ symmetry.

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Gas Transport Properties of Crosslinked Polyimide Membranes Induced by Aliphatic Diamines with Different Chain Length (사슬 길이가 다른 지방족 디아민으로 가교된 폴리이미드 분리막의 기체 투과 특성)

  • Lee, Hye Rim;Lee, Jung Moo;Nam, Sang Yong
    • Membrane Journal
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    • v.23 no.6
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    • pp.450-459
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    • 2013
  • 2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) based polyimide (PI) were crosslinked with 1,2-Diaminoethane (DAE) and 1,6-Diaminohexane (DAH) to enhance gas transport properties. Fourier transform infrared (FT-IR) studies show that imide groups were converted into amide groups during crosslinking process. Thermogravimetric analysis (TGA) results indicate that the degradation temperature of crosslinked PI membranes decreased after crosslinking. This is due to degradation of alkyl group in crosslinking agent. The d-space of crosslinked PI membranes decreased with increasing crosslinking time. The ideal permeability for $CH_4$, $N_2$, $O_2$, and $CO_2$ decreased after crosslinking and the ideal permeability of crosslinked PI membranes induced by DAH is larger than that by DAE. In contrast, the permselectivity of $CO_2/CH_4$, $CO_2/N_2$ and $O_2/N_2$ increased during crosslinking. For the gas pair of $CO_2/CH_4$, the maximum increment is about 39.5% after 6 minutes of DAE crosslinking. Also, that of $O_2/N_2$ gas pair is about 20.5% after 6 minutes of DAE crosslinking. According to these result, DAE is more suitable for enhanced permselectivity than DAH. On the contrary, DAE is not useful for $CO_2/N_2$ separation due to reduction in $CO_2/N_2$ permselectivity after 3 minutes DAE crosslinking.

Enzymatic Characterization of Peroxidase from Soybean Sprouts (콩나물 Peroxidase의 효소적 특성)

  • 박인식;이민경
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.27 no.6
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    • pp.1143-1147
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    • 1998
  • Enzymatic characterization of peroxidase(E.C. 1.11.1.7) from soybean sprouts was investigated. The optimum pH of the purified peroxidase was 7.0 and relatively stable at pH 6.0~7.0. And the optimum temperature was 50oC. The enzyme was most active with guaiacol as a substrate, followed by (+)catechin, pyrogallol and p phenylenediamine. The Km values for guaiacol and H2O2 were 4.2mM and 2.5mM, respectively. L Ascorbic acid and 2 mercaptoethanol greatly inhibited the enzyme activity, while Cu2+, Co2+ and Ni2+ activated the enzyme.

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A Qualitive Research of N2, O2 Permeation Property in PMDA/ MDA- Phenylene Diamine Copolyimide (PMDA/MDA-Phenylene diamine 계열의 공중합체막에서의 산소, 질소 투과 특성의 정성적 고찰)

  • Lee, Kyung-Rok;Na, Seong-Sun;Kim, Jong-Pyo;Min, Byoung-Ryul
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.13-19
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    • 1998
  • Copolyimide membranes of different chemical structure based on pyromellitic dianhydride (PMDA)/methylendianiline(MDA) were prepared by varying their chemical compositions with adding meta-phenylendiamine (MPD), para- phenylendiamine (PPD), 2,4,6- trimethyl-1,3-phenylenediamine(TriMeMPD) as a co-monomer. The $N_2$ and $O_2$ permeation properties are qualitatively correlated to specific free volume and intersegmental distance of membrane. The partial replacement of MDA with MPD or PPD caused in the PMDA/MDA based membranes increase in density, and decrease in free volume, d-spacing, consequently resulted in decreased permeability coefficient. In the case of TriMeMPD, opposite results were observed. In all membranes, the permeability coefficients were pressure independent, and membranes which have high permeability coefficient showed low $N_2/O_2$ ideal separation factor as an usual manner. The permeability coefficient also increased with temperature and $N_2/O_2$ ideal separation factor decreased. The increase ratio of the $N_2$ permeability coefficient was larger than that of $O_2$.

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Synthesis and Characterization of Vanadium(Ⅲ) Complexes with N, P, O-donating Ligands(Ⅱ) (질소, 산소, 인 주개 리간드를 갖는 바나듐(Ⅲ) 착물의 합성과 특성 (제 2 보))

  • Oh Sang-Oh;Lyou Eun-Young
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.612-617
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    • 1993
  • Some vanadium(III) complexes have been prepared from the reaction of VC$l_3$ with N, P, O-donating ligands and characterized by elemental analysis, $^1$H-NMR infrared and UV-Visible spectroscopy. 3,5-Lutidine, 1,2-phenylenediamine, 8-hydroxyquinoline, 9,10-phenanthrenequinone, triphenylphosphine, 1,2-bis(diphenylphosphino)ethane, 1,3-bis(diphenylphosphino)propane and 1,1'-bis(diphenylphosphino)ferrocene were chosen as coordinating ligands. Stretching frequency ${\nu}g$(V-Cl) of complexes appears) at 298∼367 cm-1, which show octahedral geometries. Stretching frequency of ${\nu}g$(V-X) (X = N, P, O) indicates that ligands are coordinated to vanadium(III). Stretching frequency ${\nu}g(C{\equiv}N)$ of acetonitrile in these complexes are characteristically shifted to about 70 c$m^{-1}$ higher compared with that of a free ligand (2260 c$m^{-1}$). Bending frequency of $\delta(C{\equiv}N)$ is also shifted to about 60 c$m^{-1}$ higher compared with that of a free ligand (377 c$m^{-1}$). Finally each vanadium(III) complex showed the following formulation; [VC$l_3$(L)$_2$MeCN] or [VC$l_3$(L-L)MeCN].

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