• The Journal of Natural Sciences
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• v.7
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• pp.47-51
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• 1995

In order to develope new asymmetric catalyst, we synthesized the following new sulfonamide derivatives start from S-Indoline-2-Carboxylic Acid via the following 5 steps. Hydroxy methyl derivative(1) was thus treated with methane sulfonyl chloride in the presence of triethylamine as base to give mesylated derivative(2) in 85% of isolated yield. The mesylate compound (2) was treated with excess sodium azide to give Azido derivative (4) in 95% isolated yield. Azido compound (3) was then reduced to the corresponding amino derivative in near quntitative yield by the hydrogenation under hydrogen atmospere in the presence of catalytic amount of Pd-C. The amino derivative (4) was converted to its sulfonamide derivatives by the treatment of compound(4) with triisopropyl benzene sulfonyl chloride in the presence of triethyl amine as base. Finally t-BOC group of the compound(5) was removed by the treatement of excess Trifluoro-acetic acid in near quantitative yield to give the target sulfonamide derivative (7) .in this paper we prepared compound(6) in 49% overall yield via the 5 steps of synthesis starting from t-Boc- 2-hydroxy methyl indoline(1) which cab be easily prepared from commercial available S-indoline-2-carboxylic acid by known methods. we plan to apply this new catalyst for the asymmetric reduction , diels-alder reaction, aldolcondensation reaction in due courses.

• Journal of the Korean Chemical Society
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• v.29 no.3
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• pp.213-219
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• 1985

The relative stability as a function of geometry in rigid cyclopropylcarbinyl cations was examined by $^{19}$F-nmr spectroscopy. 8-p-Fluorophenyl-tricyclo[3.3.1.0$^{2,7}$]octane-8-yl-(I), 9-p-fluorophenyl-tricyclo[3.3.1.0$^{2,8}$]nonane-9-yl (II), and 10-p-fluorophenyl-tricyclo[4.3.1.0$^{2,9}$]decane-10-yl cation(Ⅲ) were prepared from the corresponding carbinols in FSO$_3$H-SO$_2$ClF solution at -120$^{\circ}C$. $^{19}$F-nmr data indicate that the symmetrical bisected geometry of cyclopropane ring for ${\sigma}$-conjugation is a very impotant factor in charge delocalization. However, varied orientation of the bond angle ${\theta}$ within the bisected conformation does not affect the charge delocalization into the cyclopropane ring.

• Polymer(Korea)
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• v.28 no.4
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• pp.335-343
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• 2004

Carmustine (l,3-bis(2-chloroethyI)-1-nitrosourea, BICNU) used as antineoplastic drug for the treatment of brain tumor is not appropriate for the long term delivery, because it has short biological half life. Therefore, poly(D,L-lactide-co-glycolide) (PLGA) is useful as drug carrier for the long term delivery due to bulk erosion property. Glycolide monomer is applied to release of BICNU owing to non-toxic and monomeric components after biodegradation of PLGA. In this study, BICNU-loaded PLGA wafers with or without glycolide monomer were fabricated by conventional direct compression method for the sustained release of BICNU. These wafers were observed for their release profiles of BICNU and degradation rates by SEM, NMR, and GPC. Furthermore, we make multi-layer wafers and compare them with release profiles of conventional wafer. From these results, drug release of BICNU-loaded PLGA wafers was increased with increasing the glycolid monomer contents. We confirmed that glycolide monomer and BICNU contents in barrier-layer influenced the drug release profiles and degradation rate.

• Analytical Science and Technology
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• v.14 no.2
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• pp.159-166
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• 2001

A humic acid(HA, Aldrich Co) sample was subjected to ultrafiltration for molecular size fractionation and three fractions of different nominal size($F_1$: 1,000-10,000 daltons; $F_2$: 10,000-50,000 daltons; $F_3$: 100,000-300,000 daltons) were obtained. The structural characteristics of the size-fractionated HA were analyzed using their IR and solid state C-13 NMR spectral data, and the carboxylate group contents of the humic acids were determined using their pH titration data. The $^7F_0-{^5}D_0$ excitation spectra of Eu(III) complexes of the size-fractionated mgHA in aqueous solution were acquired($[Eu(III)]=1.0{\times}10^{-4}mol\;L^{-1}$, $(HA)=470-970mg\;L^{-1}$) at pH 5.0 using a pulsed tunable laser system, in which metal binding properties of the size-fractionated HA were elucidated and compared on another. Characterization of the IR and C-13 NMR spectral data indicated that the fraction($F_3$) with molecules of larger size were primarily aliphatic, while the fractions($F_1$, $F_2$) with smaller molecules of less than 50,000 daltons were predominantly aromatic. Titration data were consistent with an increase in the number of carboxylate groups per unit mass as molecular size became smaller. The $^7F_0-{^5}D_0$ excitation spectral data of Eu(III)-humate complexes showed that the peak maxima on these spectra were shifted toward lower energies with increasing molecular size of HA, indicating the higher degree of bindings of the Eu in the molecules of larger size. We also discussed the relationship of the lower energy shifts of the maximum peaks with increasing the molecular size of HA with the structural differences of the size-fractionated HA.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.10
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• pp.69-74
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• 2017

In this study, cholesteryl 4-n-alkoxybenzoates (Chol-n), with alkyl groups used for controlling the temperature of transition to the liquid crystal phase, were synthesized, and the effects of the length of the alkyl groups on the physical properties of the liquid crystal compounds were investigated. The chemical structures and thermal and liquid crystalline properties of the synthesized compounds were investigated by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy ($^1H$-NMR), differential scanning calorimetry (DSC), and polarizing optical microscopy (POM). The synthesized compounds showed melting transition temperatures ($T_m$) in the range of $103^{\circ}C$ to $143^{\circ}C$ and all of the compounds except Chol-6 exhibited a wide liquid crystal phase temperature range of about $60^{\circ}C$ to $100^{\circ}C$. No correlation between the number of carbon atoms in the molecule and the thermal properties of the compounds was found. All of the synthesized compounds showed an enantiotropic cholesteric phase, which was accompanied by a chiral smectic phase in the compounds Chol-6, Chol-8, Chol-9, and Chol-10. All of the compounds exhibited thermochromism in the liquid crystal state, and their color changed from red to blue as the temperature was increased.

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.441-448
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• 1986

Dioxobis(sub.-salicylaldiminato) molybdenum (VI) complexes, $MoO_2\;(X-sal-N-R)_2,\;(X=H,\;5-CH_3,\;R=C_6H_5,\;p-F-C_6H_4,\;m-Cl-C_6H_4,p-I-C_6H_4\;and\;p-C_2H_5-C_6H_4)$, have been prepared by reactions of dioxobis(sub.-salicylaldehydato) molybdenum (VI), $MoO_2(X-sal)_2$ with primary amines, in which $MoO_2(X-sal)_2$ complexes were obtained by acidification of a mixture solution of ammonium paramolybdate in water and appropriate salicylaldehyde in methanol. All these complexes show two strong Mo=O stretching imodes in the 900-940$cm^{-1}$ and p.m.r. spectra exhibited only one signal for the azomethine group. These results confirmed that the complexes are six-coordinated octahedron with a $cis-MoO_2$ group and the geometrical configurations of the complexes possess a C2 axis of symmetry. From the mass analyses of the complexes, it found that the composition ratios of $MoO_2$ : ligand are 1 : 2. The charge transfer transition corresponding to N-Mo, and O-Mo occured at 29,000$cm^{-1}$ and 32,000$cm^{-1}$ respectively. Where, the complexes were found to be non-ionic materials by conductivity measurements in dimethylformamide.

• Investigative Magnetic Resonance Imaging
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• v.12 no.2
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• pp.142-147
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• 2008

Purpose : By using the micro-imaging unit modified from NMR spectrometer, the high resolution MRI protocols of finer than 100 micron in 5 minutes, is sought for mouse, which plays a central role in animal studies Materials and Methods : C57BL/6 mouse, lighter than 50 gram, is used for the experiments. The superconducting magnet is vertical type with 89 mm inner diameter at 4.9 Tesla. The diameter of rf-coil is 30 mm. Mostly used techniques are the fast spin echo and the gradient echo pulse sequence. Results : For 2D images, proton density and T2 weighted images are obtained and their optimum experimental variables were sought. Minute structure of mouse brain can be recognized and 3D brain image is also obtained additionally. 3D image will be useful particularly for the dynamic contrast study using various contrast agents. Conclusion : Like the case of human and other small animals, the high resolution of mouse brain is enough to recognize the minute structure of it. Recently, similar studies are reported domestically, but it seems only a beginning stage. Due to easiness of breeding/control, mouse MRI study will soon play a vital part in brain study.

• Journal of the Korean Chemical Society
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• v.32 no.5
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• pp.428-435
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• 1988

Some nickel(Ⅱ) and palladium(Ⅱ) complexes of the ambidentate ligands derived from condensation of the isonitrosoacetylacetone and various diamines, $Ni(IAA)_2-en$, $Ni(IAA)_2-pn$, $Ni(IAA)_2-tn$, $Pd(IAA)_2-en$, PdCl(IAA)-pn, and $Pd(IAA)_2$-tn, where (IAA)$_2$-en, $(IAA)_2$-tn, and (IAA)-pn represent N,N'-enthylenbis(isonitrosoacetylacetone imine), N,N'-propylenebis(isonitrosoacetylacetone imine), N,N'-trimethylenebis(isonitrosoacetylacetone imine) and N-(2-aminopropyl)isonitrosoacetylacetone imine, respectively, have been prepared. The nickel(Ⅱ) and palladium(Ⅱ) complexes were characterized on the bases of the elemental analysis, IR, NMR, and electronic spectra. It is suggested that a isonitroso group of (IAA)$_2$-en or (IAA)$_2$-tn coordinates to the metal ion through the nitrogen atom to form five-membered ring, while the other isonitroso group of (IAA)$_2$-en or (IAA)$_2$-tn coordinates to the metal ion through the oxygen atom to form six membered ring in square-planar complexes of Ni(IAA)$_2$-tn and Pd(IAA)$_2$-en. And two isonitroso groups of (IAA)$_2$-en, (IAA)$_2$-pn, or (IAA)$_2$-tn coordinate to the metal ion through the nitrogen atom to form five-membered rings in square-planar complexes of Ni(IAA)$_2$-en, Ni(IAA)$_2$-pn, and Pd(IAA)$_2$-tn. On the other hand, square-planar PdCl(IAA)-pn is formed by the reaction of propylenediamine with a isonitrosoacetylacetone in the presence of palladium(Ⅱ)ion.

• Korean Chemical Engineering Research
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• v.54 no.4
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• pp.510-518
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• 2016

Ethyl cellulose-g-poly(ethylene glycol) (EP) was synthesized by esterification of carboxylic acid functionalized methoxy polyethylene glycol (MPEG-COOH) with ethyl cellulose (EC) in order to develop a hydrophilic substrate for thin-film composite (TFC) membrane in a forward osmosis (FO) system. A porous EP substrate, fabricated by a non-solvent induced phase separation method, was found to be more hydrophilic than the EC substrate due to the presence of polyethylene glycol (PEG) side chains in the EP. Since the EP substrate exhibits smaller water contact angles and higher porosity, the structural parameter (S) of TFC-EP is smaller than that of TFC-EC, indicating that internal concentration polarization (ICP) within porous substrates can occur less when TFC-EP is used as a membrane. For example, the water flux value of the TFC-EP is 15.7 LMH, whereas the water flux value of the TFC-EC is only 6.6 LMH. Therefore, we strongly believe that the TFC-EP could be a promising candidate with good FO performances.

• Analytical Science and Technology
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• v.13 no.2
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• pp.173-178
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• 2000

A new open-chain ligand containing two phenol groups, 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) was synthesized as its tetrahydrochloride salt and characterized by elemental analysis, mass, infrared and NMR. Its proton dissociation constants ($logK^n{_H}$) and stability constants ($logK_{ML}$) toward $Co^{2+}$, $Ni^{2+}$, $Cu^{2+}$ and $Zn^{2+}$ were determined at $25^{\circ}C$ and 0.10M($KNO_3$) ionic strength in aqueous solution by potentiometry. The X-ray structure of its copper (II) complex [Cu(bsated)]$(ClO_4)_2$ was reported: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. Electrochemical studies of [Cu(bsated)]$(ClO_4)_2$ complex in dimethyl sulfoxide (DMSO) solution containing tetrabutylammonium perchlorate (supporting electrolyte) were carried out by cyclic voltammograms (CV) and normal pulse voltammetry (NPV).