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Synthesis of Chloral-2-acetothienone and Trichloroethylidene-2-acetothienone, and Reaction of Trichloroethylidene-2-acetothienone with Hydrazines (Chloral-2-acetothienone과 Trichloroethylidene-2-acetothienone의 합성 및 Trichloroethylidene-2-acetothienone 과 Hydrazien 들과의 반응)

  • Lee, Hyo Won;Lee, Youn Young
    • Journal of the Korean Chemical Society
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    • v.19 no.1
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    • pp.38-42
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    • 1975
  • Chloral-2-acetothienone was synthesized from the condensation of 2-acetothienone with chloral, and trichloroethylidene-2-acetothienone was obtained from the dehydration of chloral-2-acetothienone. From the reaction of trichloroethylidene-2-acetothienone with phenylhydrazine or substituted phenylhydrazines 2-aryl-6-(2-thienyl)-3(2H)-pyridazinones were obtained. 3-(2-Thienyl)-5-trichloromethyl-2-pyrazoline was synthesized from the reaction of trichloroethylidene-2-acetothienone with hydrazine hydrate.

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The Explicit Expression of the Atomic Thermal Parameters (원자의 온도 매개변수의 정확한 표현)

  • William P. Jensen;Suh, Il-Hwan
    • Korean Journal of Crystallography
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    • v.9 no.2
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    • pp.149-152
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    • 1998
  • The accurate expression of the anisotropic thermal parameters is either exp (-2$π^{2}$ < $h^{2}$ $\frac{$u_x^2$}{$a^{2}$}$ + $k^{2}$ $\frac{$u_y^2$}{$b^{2}$}$ + $l^{2}$ $\frac{$u_z^2$}{$c^{2}$}$ + 2hk $\frac{$u_{x}}{a}$ $\frac{$u_{y}}{b}$ 2hl $\frac{$u_{x}}{a}$ $\frac{$u_{z}}{c}$ 2kl $\frac{$u_{y}}{b}$ $\frac{$u_{z}}{c}$ > ) with the small displacements Ux, Uy, uz, in absolute measure or exp (-2$π^{2}$ < $h^{2}$ $u_x^2$ + $k^{2}$ $u_y^{2}$ + $l^{2}$ $u_z^{2}$ + 2hk$u_{x}$ $u_{y}$ + 2hl$u_{x}$$u_{z}$ + 2kl$u_{y}$ $u_{z}$ > ) with the small displacements Ux, Uy, Uz in fractional measure.

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Synthesis of 1,2-Dodecylaminopropanediol and Its Mixing Effect with 1,2-Alkanediols as Preservatives (보존제로서 1,2-도데실아미노프로판디올의 합성 및 1,2-알칸디올 화합물의 혼합 효과)

  • Cha, Kyung-On;Kwak, Sang-Woon;Jeong, Kook-In;Kim, Young-Ho
    • Applied Chemistry for Engineering
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    • v.33 no.2
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    • pp.179-187
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    • 2022
  • In this study, the synthesis of 1,2-dodecylaminopropanediol (1,2-DDAP) having a 12 carbon chain length and an amine group was designed to improve the preservation and hydrophilicity of 1,2-alkanediol-based compounds. 1,2-DDAP was prepared by reacting dodecylamine (DDA) with 3-monochloro-1,2-propanediol (3-MCPD) in an ethanol solvent at 40 ℃, and its yield and purity were about 56% and 98%, respectively, under a reaction condition of 2 h and a DDA:3-MCPD molar ratio of 1:0.8. The antimicrobial effect of 1,2-DDAP showed the values of the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against microorganisms at concentrations of 10 to 100 times lower than those of 1,2-octanediol(1,2-ODIOL) or 1,2-decanediol (1,2-DDIOL). Based on the hydrophilic properties of 1,2-DDAP, mixed preservatives were prepared by adding small amounts of 1,2-ODIOL or 1,2-DDIOL, which are poorly soluble in water, with 1,2-DDAP. Mixed preservatives exhibited an effect of inhibiting microorganisms equal to or greater than that of 1,2-DDAP alone in antimicrobial activity tests. As a result of confirming the preservation effect in lotion (cosmetic formulation) for application, 1,2-DDAP showed similar antimicrobial activity at concentrations of 0.3 to 0.6 times lower than that of 1,2-ODIOL or 1,2-DDIOL. Therefore, it is considered that the use of 1,2-DDAP alone and the mixed use with small amounts of 1,2-ODIOL or 1,2-DDIOL can be a good alternative to preservatives in the product.

Synthesis of 2-Substituted-4-hydroxy-2H-1, 2-benzothiazine-3-carboxlic acid 1, 1-dioxides from 2-Substituted-3, 4-dihydro-2H-1, 2-benzothiazin-4-one 1, 1-dioxides (2-치환-3, 4-Dihydro-2H- 1, 2-benzothiazin-4-one 1, 1-dioxides로부터 2-치환-4-Hydroxy-2H-1, 2-benzothiazine-3-carboxylic acid 1, 1-dioxides의 합성)

  • 서정진;홍유화
    • YAKHAK HOEJI
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    • v.31 no.1
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    • pp.14-18
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    • 1987
  • 2-Substituted-3, 4-dihydro-2H-1, 2-benzothiazin-4-one 1, 1-dioxide 6 was reatced with magnesium methyl carbonate to form magnesium chelate 7, which could be hydrolized in cold hydrochloric acid solution to give 2-substituted-4-hydroxy-2H, 1, 2-benzothiazine-3-Carboxylic acid 1, 1-dioxide 2 in good yield.

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Synthesis and Spectroscopic Studies of Metal Complexes Formed in the Reaction of Metal Ions with Urea at High Temperature (높은 온도에서 Urea와 금속이온과의 반응으로 얻어진 금속 Complexes의 합성과 분광학적 연구)

  • Gaballa, Akmal S.;Teleb, Said M.;Nour, El-Metwally
    • Journal of the Korean Chemical Society
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    • v.51 no.4
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    • pp.339-345
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    • 2007
  • Urea reacts with PtCl2, H2[PtCl6]·6H2O, H2[IrCl6] and Ni(CH3CO2)2 in aqueous solution at high temperature (60-80 °C) yielding [PtCl2(Urea)]·2H2O (1), (NH4)2[PtCl6] (2), (NH4)2[IrCl6]·H2O (3) and [Ni2(OH)2(NCO)2(H2O)2] (4) complexes, respectively. In complex 1, urea coordinates to Pt(II) as a neutral bidentate ligand via amido nitrogen atoms. In complexes 2, 3 and 4 it seems that the coordinated urea molecules decompose during the reaction at high temperature and a variety of reaction products are obtained. All complexes were isolated in moderate yields as dark green (1), yellow (2), pale brown (3) and faint green (4) precipitates, respectively. The reaction products were characterized by their microanalysis, IR, 1H and 13C NMR spectra as well as thermal analysis. General mechanisms describing the formation of these complexes were suggested.

Determination of Hg22+ Ions Using a Modified Glassy Carbon Electrode with 2,2':6':2''-Terpyridine

  • Kong, Young-Tae;Bae, Yun-Jung;Shim, Yoon-Bo
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.346-350
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    • 2002
  • A glassy carbon electrode (GCE) modified with 2,2':6':2”-terpyridine (2,2':6':2”-TPR) using a spin coating method was applied for the highly selective and sensitive analysis of a trace amount of $Hg_2^{2+}$ ions. Various experimental parameters, which influenced the response of the 2,2':6':2”-TPR modified electrode to $Hg_2^{2+}$ ions, were optimized. The linear sweep and differential pulse voltammograms for the 2,2':6':2”-TPR modified electrode deposited with Hg show a well-defined anodic peak at +0.65 V (vs. Ag|AgCl). After a 25 min preconcentration time in an $Hg_2^{2+}$ ion solution (0.1 M acetate buffer, pH 5.0), differential pulse voltammetry(DPV) with 2,2':6':2”-TPR modified electrode shows a linear response between $1.0\;{\times}\;10^{-6}M\;and\;2.0\;{\times}\;10^{-7}M$. The least-square treatment of these data produce an equation of I[${\mu}A$] = 0.031 + 0.005C with r = 0.980(n = 5). The detection limit of this electrode with linear sweep voltammetry and differential pulse anodic voltammetry were $2.0\;{\times}\;10^{-6}M\;and\;8.0\;{\times}\;10^{-8}M$, respectively. The presence of Pb, Fe, Cd, Ti, Ni, Co, Mg, Al, Mn, and Zn did not interfere in the analysis of the $Hg_2^{2+}$ ion. The 2,2':6':2”-TPR modified GCE has been successfully applied in determination trace amounts of Hg in a human urine sample.

Precipitation of cations by alginate, polyguluronate and polymannuronate

  • Jeong, Dae-Yeong;Seo, Hyeong-Pil;Lee, Dong-Su;Byeon, Jae-Hyeong;Lee, Jin-U
    • 한국생물공학회:학술대회논문집
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    • 2000.11a
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    • pp.495-499
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    • 2000
  • The relative affinity of seaweed alginate, polyguluronate and polymannuronate for cations was investigated. The cations used in this study were $Ca^{2+}$, $Cd^{2+}$, $Co^{2+}$, $Cu^{2+}$, $Fe^{3+}$, $Hg^{2+}$, $Mg^{2+}$, $Mn^{2+}$, $Pb^{2+}$, $Rb^{1+}$, $Sr^{2+}$ and $Zn^{2+}$. The ability of cations to precipitated polymers was determined as the relative affinity of seaweed alginate, polyguluronate and polymannuronate for cations. The relative affinity of polymers for cations in order are as follow: Seaweed alginate: $Fe^{3+}$,$Cu^{2+}$,$Cd^{2+}>Pb^{2+}>Co^{2+}$,$Zn^{2+}>Ca^{2+}>Sr^{2+}$,$Rb^{1+}>Mn^{2+}>Mg^{2+}$,$Hg^{2+}$ Ployguluronate:$Fe^{3+}$,$Cu^{2+}$,$Cd^{2+}>Ca^{2+}$,$Co^{2+}$,$Pb^{2+}>Sr^{2+}$,$Rb^{1+}$,$Zn^{2+}>Hg^{2+}$,$Mn^{2+}>Mg^{2+}$ Polymannuronate:$Fe^{3+}$,$Cd^{2+}$,$Cu^{2+}>Ca^{2+}$,$Pb^{2+}>Zn^{2+}$,$Rb^{1+}$$Sr^{2+}$,$Hg^{2+}>Co^{2+}>Mn^{2+}>Mg^{2+}$

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Two New closo- or nido-Carborane Diphosphine Complexes: Synthesis, Characterization and Crystal Structures

  • Kong, Lingqian;Zhang, Daopeng;Su, Fangfang;Li, Dacheng;Dou, Jianmin
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2249-2252
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    • 2011
  • Two new carborane complexes containing closo- or nido-carborane diphosphine ligands with the formula: complex $[Hg(7,8-(PPh_2)_2-7,8-C_2B_9H_{10})_2]$ $CH_2Cl_2$ (1) and $[Ag_2({\mu}-Cl)_2(1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10})_2]$ (2) have been synthesized and characterized by elemental analysis, 1H and 13C NMR spectroscopy and X-ray structure determination. The X-ray structure analyses revealed that the carborane diphosphine ligand was degraded from closo-1,2-$(PPh_2)_2-1,2-C_2B_{10}H_{10}$ to nido-[$7,8-(PPh_2)_2-7,8-C_2B_9H_{10}]^-$ in complex 1, while the closo nature of the starting ligand $1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10}$ was retained in complex 2. In either of the two complexes, the carborane diphosphine ligand was coordinated bidentately to the Hg(II) or Ag(I) center through its two phosphorus atoms, therefore forming a five-member cheating ring between the carborane ligand and the metal center. The coordination geometry of the metal atom is distorted tetrahedron formed by $P_4$ unit in complex 1 and $P_2Cl_2$ unit in complex 2, respectively.

Microstructures and Mechanical Properties of $Al_2O_3$-$ZrO_2$ Ceramics Prepared by a Precipitation Method (침전법으로 제조한 $Al_2O_3$-$ZrO_2$계 세라믹스의 미세구조 및 기계적 특성)

  • 홍기곤;이홍림
    • Journal of the Korean Ceramic Society
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    • v.27 no.8
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    • pp.991-1003
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    • 1990
  • A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent, various types of metal hydroxides were obtained by single precipitation(series A) and co-precipitation(series B) method at the pH condition between 7 and 11. Fine Al2O3-ZrO2 powders were prepared at optimum calcination condition and the effects of ZrO2 on microstructures and mechanical properties of Al2O3 were investigated. The composition of Al2O3/ZrO2 composites wax fixed as Al2O3-15 v/o ZrO2(+3m/o Y2O3). ZrO2 limited the grain growth of Al2O3 and increased grain size homogeneity of Al2O3 more effectively than MgO.Flexural strength values in Al2O3 and Al2O3/ZrO2 composites were 340-430 MPa and 540-820 MPa, respectively, and the effect of strength improvement showed 20-50% by adding ZrO2 to Al2O3. Fracture toughness of Al2O3/ZrO2 composites was improved by stress-induced phase transformation of tetragonal ZrO2 and toughening effect by microcrack was not observed. Also, ZrO2 particles located at Al2O3 grain junction contributed to toughening, while spherical ZrO2 particles located within Al2O3 grain did not contribute to toughening. Weibull moduli of Al2O3 ceramics and Al2O3/ZrO2 composites of series A and series B were 4.34, 5.17 and 9.06, respectively. Above 0.5 of failure probability, strength values in Al2O3 ceramics and Al2O3/ZrO3 composites of series A and series B were above 400 MPa, 700 MPa and 650 MPa, respectively.

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Oxidation of trans-[FeH(NCS(Me)-S)(dppe)2]I to trans trans-[FeNCS)2(Ph2P(O)CH2CH2P(O)Ph2)2][I3](dppe=PPh2CH2CH2PPh2) (trans-[FeH(NCS(Me)-S)(dppe)2]I 화합물의 trans-[FeNCS)2(Ph2P(O)CH2CH2P(O)Ph2)2][I3]로 산화)

  • Lee, Ji Hwa;Lee, Soon W.
    • Journal of the Korean Chemical Society
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    • v.44 no.4
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    • pp.311-315
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    • 2000
  • The Fe(II)-isothiocyanato complex $trans-[FeH(NCS)(dppe)_2]$ (1) eactedwith iodomethane(Mel) to give methyl isothiocyanide-Fe(n) complex, $trans-FeH(NCS(Me)-S)(dppe)_2]I(2)$. Compound 2 was oxidized to $trans-[Fe(NCS)_2(Ph_2P(O)CH_2CH_2P(O)Ph_2)_2][I_3]$ (3), which was structurally characterized by X-ray diffraction. The molecular structure of 3 showed a bent Fe-NCS group, Crystallographic data for 3: triclinic space group P1,a=11.071(2) A,b=12.054(2)A,c=12.121(1)A, $\alpha=101.02(1){\circ}C{\beta}=95.887(9){\circ}Cr=110.34(1){\circ}C$, $Z=1R(wR_2)=0.0567(0.1294)$.

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