• Title/Summary/Keyword: $H^1$-NMR spectra

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Synthesis of Novel Polythiol for Plastic Optical Lens and its Ophthalmic Lens

  • Jang, Dong-Gyu;Roh, Soo-Gyun;Kim, Jong-Hyo;Jin, Wen-Yi;Seo, Jin-Moo;Kwon, Myeong-Ja;Lee, Soo-Min
    • Bulletin of the Korean Chemical Society
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    • v.30 no.10
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    • pp.2227-2232
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    • 2009
  • Novel polythiol materials of urethane lens series for plastic optical lens were synthesized from polyol materials via thioisouronium of thiourea with c-HCl in refluxing aqueous solution, in which polythiol material was carried out from hydrolysis of thioisouronium by ammonia water. Their structure properties were identified by EA, EI-MS, FT-IR, $^1H\;and\;^{13}C$ NMR spectroscopies and TGA. Their ophthalmic lenses as polythiourethane material were prepared by thermal curing to an injected glass mold using the evenly solutions of diisocyanates series (TDI, XDI, HDI or IPDI) with polythiols. Polythiourethane shows that the strong stretching mode for SH group of polythiol disappeared in FT-IR spectra after thermosetting polymerization. Thermal deformation starting temperature of ophthalmic lenses was determined by TMA. Ophthalmic lenses made from characteristic polythiol and diisocyanate series have transparency, colorless and good impact strength, in which thermal resistance and impact strength of ophthalmic lenses were influenced by diisocyanate series. Physical properties of ophthalmic lens have contrast thermal resistance with impact strength. The property of thermal resistance and impact strength for respective ophthalmic lenses was examined by TMA and drop ball test.

Ovicidal Activity of Lactic Acid Produced by Lysobacter capsici YS1215 on Eggs of Root-Knot Nematode, Meloidogyne incognita

  • Lee, Yong Seong;Naning, Kyaw Wai;Nguyen, Xuan Hoa;Kim, Sun Bae;Moon, Jae Hak;Kim, Kil Yong
    • Journal of Microbiology and Biotechnology
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    • v.24 no.11
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    • pp.1510-1515
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    • 2014
  • Lysobacter capsici YS1215 isolated from soil previously showed nematicidal potential for biological control of the root-knot nematode. In this study, lactic acid, a nematicidal compound, was isolated from culture filtrate of YS1215, and its ovicidal activity was investigated. Purification and identification of lactic acid were performed by a series of column chromatographies and identified by $^1H$ and $^{13}C$ NMR spectra and GC-MS analysis. Our results showed that bacterial culture filtrate containing lactic acid significantly inhibited egg hatching. The lowest egg hatch rate (5.9%) was found at a high concentration ($25 {\mu}l/ml$) of lactic acid at 5 days after incubation, followed by 20 (15.2%), 15 (23.7%), 10 (29.8%), and $5(36.4%){\mu}l/ml$, while egg hatching in the control (sterile distilled water) was 44.5%. This is the first report of lactic acid as an ovicidal compound, and it may be considered as an alternative of chemical pesticide against root-knot nematodes.

Effect of Extract from Paeoniae radix on Rabbit Platelets (작약 추출물의 혈소판 작용에 관한 연구)

  • 박영현;손동주
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.3
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    • pp.511-515
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    • 2002
  • Paeoniae radix has been considered as one of the most important crude drugs used in traditional oriental medicine and has been employed as a circulatory tonic in care of weakness, night sweats, and lumbar pain, etc. Platelet activation plays an important role in thrombosis and haemostasis. Active compounds for the inhibition of platelet activation from Paeoniae radix were extracted and fractionated into five fractions. Its fraction two and three of ethyl acetate extract inhibited the aggregation of washed rabbit platelets induced by collagen. Two active compounds, bezoyloxypaeoniflorin and paeoniflorin, were isolated from fraction two and three by silica gel column and high performance liquid chromatography. The chemical structures were determined by comparison of their proton and carbon nuclear magnetic resonance spectra. Benzoyloxypaeoniflorin showed strong inhibition at the concentration of 100 ug/mL against collagen-induced washed rabbit platelets aggregation. It is suggested that Paeoniae radix has become food material to prevent a cardiovascular disease.

Synthesis and Antitumor Evaluation of N-Alkyl-N-Nitrosocarbamoyl-$\alpha$-Amino- and 3$\beta$-Amino-$\alpha$-Cholestane Derivatives (N-Alkyl-N-Nitrosocarbamoyl-3$\alpha$-Amino-와 3$\beta$-Amino-5$\alpha$-Cholestane 유도체들의 합성 및 항암작용 평가)

  • 김정균;최순규;조인섭;유동식;유성호;문경호
    • YAKHAK HOEJI
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    • v.29 no.2
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    • pp.62-69
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    • 1985
  • The isomeric intermediates, $3{\alpha}$and $3{\beta}-amino-5{\alpha}-cholestane required for the synthesis of N-nitrosoureas, N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\alpha}-amino-5{\alpha}$-cholestane (9), N-methyl-N-nitrosocarbamoyl-3${\alpha}-amino-5{\alpha}-cholestane$ (10), N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$: (7), and N-methyl-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$ (8) were obtained through the $LiAlH_{4}$ reduction of $5{\alpha}$-cholestan-3-one oxime, followed by the chromatographic separation: the assignment of the stereochemistry of both isomers were based on the shape and chemical shift of $C_{3}$-proton resonances on their NMR spectra and on the elution mobility on the TLC. The urea intermediates, N-(2-chloroethyl) carbamoyl-3.alpha.-amino-5.alpha.-cholestane (13), N-methylcarbamoyl-$3{\alpha}-amino-5{\alpha}-cholestane$ (14), N-(2-chloroethyl) carbamoyl-$3{\beta}-amino-5{\alpha}-cholestane (11) and N-methyl-$3{\beta}-amino-5{\alpha}$-cholestane (12) were prepared by the treatment of each isomers ($3{\alpha}$-amino-and $3{\beta}-amino-5{\alpha}$-cholestane) with alkyl isocyanates in anhydrous $CHCl_{3}$, and the corresponding nitrosoureas, 7-10 were obtained by the nitrosation of the ureas, 11-14, with AcOH (or HCOOH)/$NaNO_{2}$ in ice-cold condition. The inhibitory activity of the nitrosoureas, 7-10, and their intermediates, 12-14 towards the growth of L1210 murine leukemia cells, were examined. Among them, the compounds 9 and 10 exhibited high activity having $ED_{50}$ to be 5.5g/ml and 6.1g/ml, respectively.

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Thermal and Physical Properties of Poly(butylene succinate)/Poly(${\varepsilon}$-caprolactone) Copolyesters Prepared by Transesterification (에스테르 교환반응으로 제조된 Poly(butylene succinate)/Poly(${\varepsilon}$-caprolactone) Copolyesters의 물리적 및 열적 성질에 관한 연구)

  • Yoo, Young-Tai;Yang, Su-Bong;Im, Seung-Soon
    • Polymer(Korea)
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    • v.25 no.4
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    • pp.486-495
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    • 2001
  • Degradable poly(butylene succinate) (PBS)/poly(TEX>${\varepsilon}$-caprolactone) (PCL) copolyesters were prepared by using transesterification between poly(butylene succinate) and poly(TEX>${\varepsilon}$-caprolactone). The thermal and mechanical properties of copolyesters were investigated using differential scanning calorimetry and tensile testing. Interchange reaction between PBS and PCL molecules could be identified from proton NMR spectra. The reduced viscosity of the PBS/PCL copolyesters increased with reaction time except for a series of PBS/PCL (50/50 wt%) copolyesters. For all the compositions, the melting point and crystallization temperature of high-$T_m$ component (PBS) decreased as reaction time increased. From the results of tensile testing, it was found that stress and strain at break of the PBS/PCL copolymers containing less than 40 wt% PCL improved as compared to those of pure PBS, but at 50 wt% PCL stress at break of PBS/PCL copolymers was lowered due to decrease of crystallinity. On the other hand, Young's moduli of all the copolyesters decreased with both reaction time and PCL content.

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A Study on the Fouling of Ultrafiltration Membranes Used in the Treatment of an Acidic Solution in a Circular Cross-flow Filtration Bench (순환식 막 모듈 여과장치를 이용한 산성용액의 수처리 공정 시 발생하는 한외여과막 오염에 관한 연구)

  • Kim, Nam-Joon;Choi, Chang-Min;Choi, Yong-Hun;Lee, Jun-Ho;Kim, Hwan-Jin;Park, Byung-Jae;Joo, Young-Kil;Kang, Jin-Seok;Paik, Youn-Kee
    • Membrane Journal
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    • v.19 no.3
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    • pp.252-260
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    • 2009
  • The effects of the treatment of an acidic solution at pH 2 on polyacrylonitrile ultrafiltration (UF) membranes were investigated using a circular cross-flow filtration bench with a membrane module. A substantial reduction in the membrane permeability was observed after 80 hours' treatment of the acidic solution. In addition, the analyses of the sample solutions by ultraviolet/visible absorption spectroscopy and gas chromatography/mass spectrometry (GC/MS), which were taken from the feed tank as a function of the treatment time, showed that a new organic compound was produced in the course of the treatment. From a thorough search of the mass spectral library we presumed the new compound to be 1,6-dioxacyclododecane-7,12-dione (DCD), one of the well-known additives for polyurethane. Based on further experimental results, including the scanning electron microscope (SEM) images and the solid-state NMR spectra of the membranes used for the treatment of the acidic solution, we suggested that the decrease of the permeate flux resulted not from the deformation of the membranes, but from the fouling by DCD eluted from the polyurethane tubes in the filtration bench during the treatment. Those results imply that the reactivity to an acidic solution of the parts comprising the filtration bench is as important as that of the membranes themselves for effective treatments of acidic solutions, for efficient chemical cleaning by strong acids, and also in determining the pH limit of the solutions that can be treated by the membranes.

Neurochemical Profile Quantification of Regional Adult Mice Brain Using: ex vivo $^1H$ High-Resolution Magic Angle Spinning NMR Spectroscopy (생체 외 조직 고 분해능 Magic Angle Spinning을 이용한 정상 Adult Mice에서의 뇌 부위별 뇌 신경화학 대사물질 정량분석)

  • Lee, Do-Wan;Woo, Dong-Cheol;Lee, Sung-Ho;Kim, Sang-Young;Kim, Goo-Young;Rhim, Hyang-Shuk;Choi, Chi-Bong;Kim, Hwi-Yool;Lee, Chang-Wook;Choe, Bo-Young
    • Progress in Medical Physics
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    • v.21 no.1
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    • pp.35-41
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    • 2010
  • The purpose of this study is to quantitate regional neurochemical profile of regional normal adult mice brain and assess regional metabolic differences by using ex vivo $^1H$ high-resolution magic angle spinning nuclear magnetic resonance spectroscopy ($^1H$ HR-MAS NMRS). The animals were matched in sex and age. The collected brain tissue included frontal cortex, temporal cortex, thalamus, and hippocampus. Quantitative 1D spectra were acquired on 40 samples with the CPMG pulse sequence (8 kHz spectral window, TR/TE = 5500/2.2 ms, NEX = 128, scan time: 17 min 20 sec). The mass of brain tissue and $D_2O$+TSP solvent were 8~14 mg and 7~13 mg. A total of 16 metabolites were quantified as follow: Acet, NAA, NAAG, tCr, Cr, tCho, Cho, GPC + PC, mIns, Lac, GABA, Glu, Gln, Tau and Ala. As a results, Acet, Cho, NAA, NAAG and mIns were showed significantly different aspects on frontal cortex, hippocampus, temporal cortex and thalamus respectively. The present study demonstrated that absolute metabolite concentrations were significantly different among four brain regions of adult mice. Our finding might be helpful to investigate brain metabolism of neuro-disease in animal model.

Synthesis and Properties of Molybdenum and Tungsten Oxo-Nitrosyl Complexes of Methylthioamidoxime (산소-니트로실 착물의 연구(제3보): 티오메틸아미드옥심의 몰리브덴과 텅스텐 산소-니트로실 착물의 합성과 특성)

  • Roh, Soo Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.40 no.1
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    • pp.28-36
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    • 1996
  • The pentanuclear complexes have been obtained by the reactions of molybdenum(VI) and tungsten(VI) polynuclear complexes with molybdenum(O) and tungsten(O) dinitrosyl mononuclear complexes, and methylthioamidoxime. The prepared complexes (n-Bu4N)2[Mo4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](1), (n-Bu4N)2[W4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](2), (n-Bu4N)2[Mo4O12W (NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] (3) have been characterized by elemental analysis, infrared, UV-visible and 1H NMR spectra. The complexes are elucidated the cis-{M(NO)2}2+(M = Mo, W) unit and a slight delocalization by spectroscopy. The structure of (n-Bu4N)2[W4O12Mo(NO) 2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P21}a$, a = 22.14(2) $\AA$, b = 14.93(1) $\AA$, c = 23.20(1) $\AA$, $\beta$ = 111.08(6) $\AA$, V = 7155(9) $\AA$, Z = 4, final R = 0.072 for 6191(I > $3\sigma(I)).$ The structure of complex forms two dinuclear [W2O5{CH3SCH2C(NH2)NHO}{CH3SCH2C(NH)NO}] and a central {Mo(NO)2} 2+ core. The geometric structure of the {Mo(NO)2} 2+unit is the formally cistype and C2v symmetry.

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Isolation and HPLC Analysis of Timosaponin A III from Rhizomes of Anemarrhena asphodeloides $B_{UNGE}$ (지모의 유효성분 분리 및 HPLC 정량 분석)

  • Kim, Geum-Soog;Park, Chang-Kie;Seong, Jae-Duck;Kim, Hyun-Tae;Han, Sang-Ik;Kwack, Yong-Ho
    • Korean Journal of Medicinal Crop Science
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    • v.7 no.1
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    • pp.45-50
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    • 1999
  • Timosaponin A III, an active and major compound, was isolated from rhizomes of Anemarrhena asphodeloides. The quantitative analysis of timosaponin AIII was performed by a high performance liquid chromatographic(HPLC) method using ELSD and the useful extraction method for HPLC analysis was examined as well. This HPLC method can be utilized as the standard analytical method for the evaluation of the quality of Anemarrhena rhizoma in the steps of breeding and cultivation. Additionally, the HPLC analysis method can be useful for the evaluation of the quality of Anemarrhena rhizoma sold as a traditional medicine in current markets.

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