• Bulletin of the Korean Chemical Society
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• 제23권1호
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• pp.132-136
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• 2002

$Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)\;(OTf=CF_3SO_3^-)$ readily reacts with various amines to afford cationic amine complexes $[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(amine)](OTf)\;(amine=NH_3,\;NHMe_2,\;NHC_4H_8,\;NH_2Ph,\;NH_2(Tol-p))$ in high yields. These complexes have been fully characterized by IR, $^1H-,\;^{19}F{^1H}-,\;and\;^{31}P{^1H}-NMR$ spectroscopy, and elemental analyses. Reaction of $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ with acrylonitrile quantitatively produced the ${\pi}$-olefinic complex $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(CH_2=CHCN)](OTf)$ which is only stable in solution in the presence of acrylonitrile. Attempt at isolating this complex in the pure solid state was failed due to partial decomposition into $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ The equilibrium constants $(K_{eq}=[Pt(PCP)-(NH_2R)^+][CH_2=CHCN]/[Pt(PCP)(CH_2=CHCN)^+][NH_2R]:\;[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(CH_2=CHCN)]^++NH_2R{\rightleftarrows}[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(NH_2R)]^++CH_2=CHCN=Ph,\;p-tolyl)$ were calculated to be 0.28 (for R = Ph) and 3.1 (R = p-tolyl) at $21^{\circ}C$. The relative stability of the ${\sigma}$-donor amine versus the ${\pi}$-olefinic acrylonitrile complex has been found largely dependent upon the amine-basicity $(pK_b)$, implicating that acrylonitrile practically competes with amine in the platinum coordination sphere. On the contrary to the formation of the acrylonitrile complex, no reaction of $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ with other olefins such as ethylene, styrene and methyl acrylate was observed.

• Polymer(Korea)
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• 제39권3호
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• pp.487-492
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• 2015

The effects of chemical structure of alkyl groups of norbornene carboxylic alkyl esters(methyl, octyl, 4-chlorobenzyl) and endo/exo ratios of norbornene monomers on activity of palladium catalyst and polymerization behavior were investigated. Norbornene ester monomers were synthesized from the reaction of 5-norborene-2-carboxylic acid and various alcohols. Polymerization catalyst, di-${\mu}$-chloro-bis(-methoxybicyclo[2,2,1]-hept-2-ene)palladium(II) (DCBMP), was synthesized according to the literature procedure and silver hexafluoroantimonate ($AgSbF_6$) was used as a conjugate anion source. Gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) were the principal techniques for polymer characterization and $^1H$ NMR spectroscopy was used for chemical structures determination of monomers and polymers. For all of the norbonene alkyl esters GPC data showed that when the amounts of endo isomers exceeded those of exo isomers decreased molecular weight polymers were obtained probably due to the decreased catalyst activity. Polymerizations were conducted by varying the monomer/catalyst mole ratios (100:1, 200:1, 300:1). When 300:1 monomer/catalyst ratio was employed it was possible to synthesize high molecular weight ($M_n=27500g/mol$), film forming polymer from exo-norbornene carboxylic acid octyl ester.

• Bulletin of the Korean Chemical Society
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• 제16권6호
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• pp.524-528
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• 1995

The reaction of [IrCl(cod)]2 with ppol ligand, Ph2PCH2CH2CH2P(Ph)CH2CH2CH=CH2, in ethanol gives an iridium complex, whose structure is converted from an ionic form, [Ir(cod)(ppol)]Cl·2C2H5OH (1),in polar solvents (ethanol, methanol and acetonitrile), to a molecular form, [IrCl(cod)(ppol)], in non-polar solvents (benzene and toluene). The cationic complexes, [Ir(cod)(ppol)]AsF6·1/2C2H5OH and [Ir(cod)(ppol)]PF6·1/2CH3CN, were prepared to compare with the ionic form by 31P NMR spectroscopy. When carbon monoxide is introduced to 1, cod is replaced by CO to give the 5-coordinated complex, [IrCl(CO)(ppol)]. Hydrogenation of 1-octene was not successful in the presence of 1. In order to verify the reason for 1 not behaving as a good catalyst for hydrogenation, electrophilic reactions with HCl, I2 and HBF4·etherate were performed, which yielded the oxidative addition product, [IrHCl2(ppol)], the substitution product, [IrI(cod)(ppol)], and another cationic product, [Ir(cod)(ppol)]BF4, respectively. Thus, the iridium complex is not sufficiently basic to activate hydrogen atoms or the olefin of the ppol ligand.

• Bulletin of the Korean Chemical Society
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• 제32권6호
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• pp.2021-2026
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• 2011

AgNPs (silver nanoparticles) has been widely used for the commercial products, which have antimicrobial agent, medical devices, food industry and cosmetics. Despite, AgNPs have been reported as toxic to the mammalian cell, lung, liver, brain and other organs and many researchers have investigated the toxicity of AgNPs. In this study, we investigated toxicity of the AgNPs to the liver cell using metabolomics based on HRMAS NMR (High Resolution Magic Angle Spinning Nuclear Magnetic Resonance) technics, which could apply to the intact tissues or cells, to avoid the sample destruction. Target profiling and multivariative statistical analysis were performed to analyze the 1D $^1H$ spectrum. The results show that the concentrations of many metabolites were affected by the AgNPs in the liver cell. The concentrations of glutathione (GSH), lactate, taurine, and glycine were decreased and most of amino acids, choline analogues, and pyruvate were increased by the AgNPs. Moreover, the levels of the metabolites were recovered upto similar level of metabolites in the normal cell by the pre-treatment of NAC, external antioxidant. The results suggest that the depletion of the GSH by the AgNPs might induce the conversion of lactate and taurine to the pyruvate.

• Journal of the Korean Society of Food Science and Nutrition
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• 제44권7호
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• pp.1090-1099
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• 2015

Among the four different parts of mulberry (Morus alba L.) tree, ethanol extract of Morus root bark showed the highest ${\alpha}$-glucosidase inhibitory activity ($IC_{50}=12.01{\mu}g/mL$). Bioassay-guided fractionation of the ethanolic extract of root bark by Diaion HP-20, silica gel, ODS-A, and Sephadex LH-20 column chromatographies led to the isolation of four compounds, including Compound (Comp.) 1 ($IC_{50}=5.22{\mu}g/mL$), Comp. 2 ($IC_{50}=1.78{\mu}g/mL$), Comp. 3 ($IC_{50}=2.94{\mu}g/mL$), and Comp. 4 ($IC_{50}=1.54{\mu}g/mL$) with strong ${\alpha}$-glucosidase inhibitory activities. Their chemical structures were elucidated as morusin (Comp. 1), kuwanon H (Comp. 2), chalcomoracin A (Comp. 3), and chalcomoracin B (Comp. 4) by UV and NMR spectral analyses. These results suggest that prenylflavonoid and mulberrofuran of Morus root bark may be useful as potential therapeutic agents for diabetes.

• Macromolecular Research
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• 제17권10호
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• pp.770-775
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• 2009

$\omega$-Anhydride-functionalized poly(ethylene oxide) (PEO) obtained from chain-end functionalization and anionic ring-opening polymerization of ethylene oxide using n-butyllithium with potassium t-butoxide in the presence of dimethylsulfoxide (DMSO) was found to be an efficient material for the preparation of water-soluble, polymeric pro-drugs. The reaction of $\omega$-anhydride-functionalized PEO with sulfonamide or with vancomycin provided an efficient method to produce corresponding, water-soluble, PEO-conjugated sulfonamide or PEO-conjugated, vancomycin pro-drugs. These were used successfully to prepare water-dispersible, silver nanoparticles. In this study, the particle sizes were in the range of $5{\sim}40$ nm. The resulting products were characterized by $^1H$ NMR spectroscopy, transmission electron microscopy, electron and X-ray diffraction, size exclusion chromatography, and UV/Visible spectroscopy.

• Macromolecular Research
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• 제17권5호
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• pp.301-306
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• 2009

This work has demonstrated that a novel amphiphilic poly(epichlorohydrine)-graft-polystyrene (PECH-g-PS) copolymer at 34:66 wt% was synthesized via atom transfer radical polymerization (ATRP) of styrene using PECH as a macroinitiator. The structure of the graft copolymer was characterized by nuclear magnetic resonance ($^1H$ NMR) and FTIR spectroscopy, demonstrating that the "grafting from" method using ATRP was successful. The self-assembled graft copolymer was used as a template film for the in-situ growth of silver nanoparticles from $AgCF_3SO_3$ precursor under UV irradiation. The in situ formation of silver nanoparticles with 6-8 nm in average size in the solid state template film was confirmed by transmission electron microscopy (TEM), UV-visible spectroscopy and wide angle X-ray scattering (WAXS). Differential scanning calorimetry (DSC) also displayed the selective incorporation and the in situ formation of silver nanoparticles within the hydrophilic PECH domains, probably due to stronger interaction of the silvers with the ether oxygens of PECH backbone than that with hydrophobic PS side chains.

• Bulletin of the Korean Chemical Society
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• 제32권7호
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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.

• Journal of the Korean Applied Science and Technology
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• 제38권2호
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• pp.476-487
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• 2021

To prepare acrylic resin coatings containing 70% of solids, we used n-butyl methacrylate(BMA), methyl methacrylate(MMA), 2-hydroxyethyl methacrylate(2-HEMA), and acetoacetoxyethyl acrylate(AAEA), caprolactone acrylate(CLA) as raw materials, the glass transition temperature(T_g) of acrylic copolymer was adjusted around 50 ℃. The viscosity and molecular weight of the acrylic resins was increased with increasing OH values. Di-tert-amyl peroxide was found to be the suitable initiator to get high-solids acrylic resins. The optimum reaction conditions found in the study are 5 wt% of initiator, 4 wt% of chain transfer agent, 4 hrs of dropping time, and 140 ℃ of reaction temperature. The structure of the synthesized resins were characterized by FT-IR and ¹H-NMR spectroscopy. Number average molecular weight of 1900~2600 and molecular wight distribution of 1.4~2.1 were obtained. Crosslinked acrylic urethane clear coatings were obtained by curing reaction between the synthesized acrylic resins and hexamethylene diisocyanate trimer(Desmodur N-3300), the equivalent ratio of NCO/OH was 1.2/1.0. The physical properties from the following studies were carried out: viscosity(Zahn cup #2), adhesion, drying time, pot-life, pensil hardness, and 60° specular gloss. Various properties of the acrylic urethane clear coatings were also evaluated on the coating specimens. Adhesion property to a substrate, drying time, pot-life, pencil hardness, and 60° specular gloss of prepared paint showed quite good properties. Futhermore, prepared paint containing 10% of CLA showed quite good properties for adhesion, low viscosity and high hardness.

• Journal of the Korean Chemical Society
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• 제42권2호
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• pp.184-189
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• 1998

Tris(pentafluorophenyl)indium acetonitrile complexes have been prepared from the reaction of Indium trihalides (halogen=Cl, Br) and bis(pentafluorophenyl)cadmium in acetonitrile, and characterized by elementary analysis, $^13C{^1H}-,\; ^1H-\;and\; ^{19}F-NMR$ spectroscopy and mass spectrometry. The Indium (III) compounds were formed stable 1:1 adducts with acetonitrile. $In(C_6F_5)_3{\cdot}DMAP$ has been prepared from the ligand exchange reaction of In$(C_6F_5)_3 {\cdot} CH_3CN$ with DMAP in $CH_2Cl_2 {\cdot} DMAP$ has higher donating character and replaced the $CH_3CN$ through the ligand transfer reaction.