• Title/Summary/Keyword: NMR 분광법

Search Result 148, Processing Time 0.027 seconds

Synthesis and Properties of Anionic Tetrakis(pentafluorophenyl)indium(Ⅲ) Complexes (Tetrakis(pentafluorophenyl)indium(Ⅲ) 음이온 착물의 합성과 특성)

  • Choi, Zel Ho
    • Journal of the Korean Chemical Society
    • /
    • v.43 no.1
    • /
    • pp.52-57
    • /
    • 1999
  • The anionic complexes, [ln($C_6F_5)_4$]-, which are thermal and moisture sensitive, have been prepared by the reaction of In($C_6F_5)_3{\cdot}D(D=CH_3CN$, O($C_2H_5)_2$) with the system ($CH_3)_3SiC_6F_5$/CsF, $C_6F_5$MgBr or Cd($C_6F_5)_2$. The stable anionic indium(III) complexes are obtained through cation exchange with PNPCI ([PNP]= bis(triphenylphosphino)ammonium). The pure substance is obtained by column chromatography. These new anionic complexes are unambiguously identifed by NMR-spectroscopy, IR spectroscopy, molecular weight, DTA/TG and elemental analysis.

  • PDF

Analysis of Tridentate Schiff Base Ni(II) Complex (세자리 Schiff Base의 Ni(II) 착물의 분석)

  • Chae, Hee-Nam;Choi, Yong-Kook
    • Analytical Science and Technology
    • /
    • v.11 no.5
    • /
    • pp.332-340
    • /
    • 1998
  • Tridentate Schiff base ligands, $SIPH_2$, $SIPCH_2$, $HNIPH_2$, and $HNIPCH_2$ were prepared by the reactions of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with 2-aminophenol and 2-amino-p-cresol. Ni(II) complexes of those ligands were synthesized. The structures and properties of ligands and their complexes were studied by elemental analysis, $^1H$-NMR, IR, UV-visible spectra, and thermogravimetric analysis. The mole ratio of Schiff base to the metal of complexes was found to be 1:1. Ni(II) complexes were contemplated to be hexa-coordinated octahedral configuration containing three water molecules. The redox process of ligands and complexes in DMSO solution containing 0.1 M TBAP as supporting electrolyte was investigated by cyclic voltammetry and differential pulse voltammetry with glassy carbon electrode. The redox process of the tridentate Schiff base ligands was totally irreversible. The redox process of Ni(II) complexes were quasi-reversible and diffusion-controlled as one electron by one step process Ni(II)/Ni(I). The reduction potentials of the Ni(II) complexes shifted in the positive direction in the order [$Ni(II)(HNIP)(H_2O)_3$]>[$Ni(II)(SIP)(H_2O)_3$]>[$Ni(II)(SIPC)(H_2O)_3$]>[$Ni(II)(HNIPC)(H_2O)_3$] and their dependence on ligands were not so high. Consequently the [$Ni(II)(HNIPC)(H_2O)_3$] complex among the synthesized Ni(II) complexes was found to be most stable in the DMSO solution.

  • PDF

A Green Preparation of Drug Loaded PAc-β-CD Nanoparticles from Supercritical Fluid (초임계 유체를 이용한 약물이 담지된 PAc-β-CD 나노 입자의 친환경적인 제조)

  • Jang, Min Ki;Kim, Yong Hun;Kim, Dong Woo;Lee, Si Yun;Lim, Kwon Taek
    • Clean Technology
    • /
    • v.26 no.1
    • /
    • pp.1-6
    • /
    • 2020
  • Rapid expansion of supercritical solution (RESS) process was used to make molsidomine (MOL) loaded peracetyl-β-cyclodextrin (PAc-β-CD) nanoparticles, which were collected into the air. The effect of the concentration of the drug PAc-β-CD (0.5 and 1 wt%), extraction temperature (45 ~ 60 ℃), nozzle length (5 ~ 20 mm) and internal diameter (ID) (50 ~ 150 μm) of a capillary, and spray distance on the particle size and morphology of the resulting particles were investigated. The interaction of a drug and PAc-β-CD was confirmed by 1H-NMR spectroscopy while the particle size was measured by means of a scanning electron microscope. It was found that increasing the temperature from 45 ℃ to 60 ℃ and decreasing the nozzle diameter from 150 μm to 50 μm had an increasing effect on the average particle size, while increasing the spray distance led to a decrease in the average particle size at a constant pressure of 34.5 MPa and temperature of 45 ℃. With 0.5 wt% of PAc-β-CD, the capillary nozzle of short length (5 mm) and small ID (50 μm) gave the smallest size (165 nm). The obtained nanoparticles showed increased dispersity and solubility in oil. The oil suspension of the inclusion complex showed increased sustainability, which can increase the in-vitro controlled release time of the drug.

Molecular Structure of PCP Pincer Complexes: Poisoning Catalyst on the Dehydrogenation of Alkanes (알칸의 탈수소화반응에서의 촉매독 화합물의 분자구조)

  • Lee Ji Hyun;Chun Sang Jin;Kwon Ki Hyeok;Lee Do Weon
    • Korean Journal of Crystallography
    • /
    • v.16 no.1
    • /
    • pp.43-53
    • /
    • 2005
  • The dihydrido P-C-P pincer complex, $IrH_2{C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (1), was successfully prepared from the reaction of the hydrochloride complex, $IrClH (C_6H_3-2,6-(CH_2PBu_2^t)_2}$, and super acid $(LiBEt_3H)$ under 1 atm of hydrogen in pentane solution at room temperature and followed by Heating at $130^{\circ}C$ in vacuo. Jensen recently found that the dihydrido P-C-P pincer complex 1 is a highly active homogeneous catalyst for the transfer dehydrogenation of alkanes with unusual longterm stability at temperatures as high as $200^{\circ}C$. The treatment of dihydrido complex 1 with nitrogen, water, carbon dioxide, and carbon monoxide in presence of tert-butylethylene (the) at room temperature in an appropriate solution gave the dinitrogen complex, $[Ir{C-6H_3-2,6-(CH_2PBu_2^t)_2}]_2({\mu}-N_2)$ (2), the hydrido hydroxyl complex, $IrH(OH){C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (3), the carbon dioxide complex, $Ir({\eta}^2-CO_2) {C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (including the bicarbonate complex, $IrH({\kappa}^2-O_2COH){C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(4))$, and the carbonyl complex, $Ir(CO) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(5)$ (including the carboxyl complex, $IrH(C(O)OH) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(6))$, in good yield, respectively. These P-C-P iridium complexes were isolated and characterized by $^1H,\;^{13}C,\;^{31}P\; NMR$, and IR spectroscopy. In addition, the complexes (1-6) were characterized by a single crystal X-ray crystallography. These complexes account for these small molecules' inhibition of dehydrogenation of alkanes catalyzed by the dihydrido complex 1.

Synthesis of Tridentate-Schiff Base Co(II) Complexes and Their Electrochemical Properties (세자리 Schiff Base Co(Ⅱ) 착물의 합성과 전기화학적 성질)

  • Chae, Hui Nam;Choe, Yong Guk
    • Journal of the Korean Chemical Society
    • /
    • v.42 no.4
    • /
    • pp.422-431
    • /
    • 1998
  • Tridentate Schiff base ligands such as $SIPH_2,\;SIPCH_2,\;HNIPH_2,\;and\; HNIPCH_2$ were prepared by the reaction of salicylaldehyde and 2-hydroxy-l-naphthaldehyde with 2-aminophenol and 2-amino-p-cresol. The structures and properties of ligands and their Co(II) complexes were investigated by elemental analysis, $^1H$NMR, IR, UV-visible spectra, and thermogravimetric analysis. The molar ratio of Schiff base to the metal of complexes was found to be 1:1. Co(II) complexes were contemplated to be hexa-coordinated octahedral configuration containing three water molecules. The redox process of ligands and complexes in DMSO solution containing 0.1 M TBAP as a supporting electrolyte were investigated by cyclic voltammetry with glassy carbon electrode. The redox process of the tridentate Schiff base ligands was totally irreversible. The redox process of Co(II) complexes were irreversible and one electron processes by two steps in diffusion controlled reaction. The reduction potential of the Co(II) complexes was shifted to the positive direction in the order [Co(Ⅱ)$(HNIPC)(H_2O)_3$]>[Co(Ⅱ)$(HNIP)(H_2O)_3$]>[Co(II)$(SIPC)(H_2O)_3$]>[Co(Ⅱ)$(SIP)(H_2O)_3], and their dependence on ligands were not so high.

  • PDF

Synthesis of Transition Metal Cu(II) Complexes and Their Electrochemical Properties (Cu(II) 전이금속 착물의 합성과 전기화학적 성질에 관한 연구)

  • Chae, Hee-nam;Choi, Yong-kook
    • Applied Chemistry for Engineering
    • /
    • v.9 no.5
    • /
    • pp.719-725
    • /
    • 1998
  • Tridentate Schiff base ligands were prepared by the reactions of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with 2-aminophenol and 2-amino-p-cresol. And then Cu(II) complexes of those ligands were synthesized. The structures and properties of ligands and their complexes were studied by elemental analysis, $^1H$-NMR, IR, UV-visible spectra, and thermogravimetric analysis. The mole ratio of Schiff base to the metal of complexes was found to be 1:1. Cu(II) complexes were contemplated to be four-coordinated square planar configuration containing one water molecule. The redox process of ligands and complexes in DMSO solution containing 0.1 M TBAP as a supporting electrolyte was investigated by cyclic voltammetry and differential pulse voltammetry with glassy carbon electrode. The redox process of the tridentate Schiff base ligands was totally irreversible. The redox process of Cu(II) complexes was quasi-reversible and diffusion-controlled as one electron by one step process Cu(II)/Cu(I). The reduction potentials of the Cu(II) complexes shifted in the positive direction in the order of [Cu(II)(HNIPC)($H_2O$)]>[Cu(II)(HNIP)($H_2O$)]>[Cu(II)(SIP)($H_2O$)]>[Cu(II)(SIPC)($H_2O$)].

  • PDF

Platinum(II) Complexes of 2,2-bis(Methylaminomethyl)-1,3-dioxolane (2,2-비스(메틸아미노메틸)-1,3-dioxolane의 백금(Ⅱ) 착물)

  • Moo-Jin Jun
    • Journal of the Korean Chemical Society
    • /
    • v.22 no.2
    • /
    • pp.99-104
    • /
    • 1978
  • The synthesis of a bidentate secondary amine ligand, 2,2-bis(methylaminomethyl-2,3-dioxolane(methylaminomethyl)-1,3-dioxolane(mexo) and the preparation of dichloro and trans-R-cyclohexanediamine platinum(II) complexes of this ligand are reported. The structures of the ligand and complexes prepared have been elucidated via elemental analyses, nmr, electronic absorption, and CD spectra.

  • PDF

Synthesis and Applications of Reactive Polymer Modifiers for Asphalt(1) (아스팔트용 반응성 고분자 개질제 합성 및 적용(1))

  • Hwang, Ki-Seob;Ahn, Won-Sool;Suh, Soong-Hyuck;Ha, Ki-Ryong
    • Polymer(Korea)
    • /
    • v.31 no.1
    • /
    • pp.68-73
    • /
    • 2007
  • This study is on the synthesis of reactive polymer modifiers by emulsion polymerization to improve properties of asphalt for paving. Styrene, methyl methacrylate (MMA), isoprene and glycidyl methacrylate (GMA) which has epoxy ring to react with carboxyl group of asphaltene were used to synthesize polymer modifiers. Modifiers with various composition were tested miscibility with asphalt. Modifiers which showed good miscibility with asphalt were investigated by DSC for $T_g$. Existence of epoxy rings and their reaction with asphaltene wore investigated by FTIR. Molecular structures of synthesized modifiers were confirmed by $^1H-NMR$. The synthesized modifiers which showed good miscibility had their $Tg's$ in the range of $37.5{\sim}56.5^{\circ}C$ and had isoprene contents of 30 wt%. They showed good miscibility in the 1 and 2 wt% concentrations, but not in the 3 wt% concentration.

Quantitative Analysis of Platycodin D from Platycodon grandiflorum by HPLC-ELSD (HPLC-ELSD법에 의한 길경의 platycodin D 정량분석)

  • Kim, Geum-Soog;Kim, Hyun-Tae;Seong, Jae-Duck;Park, Hee-Saeng;Kim, Soo-Dong
    • Korean Journal of Medicinal Crop Science
    • /
    • v.10 no.3
    • /
    • pp.200-205
    • /
    • 2002
  • Platycodin D was isolated from n-butanol extract of Platycodi radix(Platycodon grandiflorum and identified by the spectroscopic analysis using $^1H$ and $^{13}C$ NMR techniques. A new method of analysis of platycodin D by high performance liquid chromatography(HPLC) was established using a reversed phase system with YMC-Pack ODS-AM( 250 X 4.6 mm) column and 30% acetonitrile as a mobile phase. Evaporative light scattering detector was used as detector. The kinds of extraction solvents and methods were examined to determine the efficient extraction condition and HPLC analysis was carried out to establish the optimum drying condition for the root of Platycodon grandiflorum. The contents of Platycodin D was highest as 0.083% when platycodon roots were dried at $60^{\circ}C$ using dry oven.

Synthesis and Characterization of Paramagnetic Copper(Ⅱ) Complexes (상자성 구리(Ⅱ) 화합물의 합성과 그 특성 연구)

  • Oh, Yeong-Hee
    • Journal of the Korean Chemical Society
    • /
    • v.44 no.6
    • /
    • pp.507-512
    • /
    • 2000
  • A new copper(II) complex, Cu(dpb)(NO$_3$)$_2$(H$_2$O) (dpb=2,2'-dipyridylbenzylamine) (1) was synthesized from the reaction of Cu(NO$_3$)$_2$·3H$_2$O and dpb in ethanol solution followed by recrystallization in acetonitrile. The structure of 1 was determined by X-ray diffraction methods. The single crystal structure was characterized as follows: space group P2$_1$/c, Z=4, a=12.501(9)$\AA$, b=9.231(10)$\AA$, c=17.119(6)$\AA$, $\alpha$=90$^{\circ}$, $\beta$=107.33(4)$^{\circ}$, $\gamma$=90$^{\circ}$, V=1885.8(2)$\AA^3$, R$_1$=0.0647, $_{w}R$_2$$=0.1866 for 3258 reflections. Compound was a typical paramagnetic copper(II) complex coordinated by 2,2'-dipyridylamine derivative ligand, which was confirmed by EPR, NMR, UV/VIS, and IR spectroscopy.

  • PDF