• Title/Summary/Keyword: $^2H$ NMR

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Syntheses of Alternating Head-to-Head Copolymers of Vinyl Ketones and Vinyl Ethers, and Their Properties. Ring-Opening Polymerization of 2,3,6-Trisubstituted-3,4-dihydro-2H-pyrans

  • Lee, Ju-Yeon;Cho, I-Whan
    • Bulletin of the Korean Chemical Society
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    • v.8 no.2
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    • pp.102-105
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    • 1987
  • 2-Methoxy-6-methyl-3,4-dihydro-2H-pyran ($1_a$), 2-ethoxy-3,6-dimethyl-3,4-dihydro-2H-pyran ($1_b$), and 2-ethoxy-3-methyl-6-ethyl-3,4-dihydro-2H-pyran ($1_c$) were prepared by (4 + 2) cycloaddition reaction from the corresponding vinyl ketones and alkyl vinyl ethers. Compounds $1_{a-c}$ were ring-open polymerized by cationic catalyst to obtain alternating head-to-head (H-H) copolymers. For comparison, copolymer of head-to-tail (H-T) was also prepared by free radical copolymerization of the mixture of the corresponding monomers. The H-H copolymer exhibited some differences in its $^1H$ NMR and IR spectra. However, significant differences were showed between the H-H and H-T copolymers in the $^{13}C$ NMR spectra. Also noteworthy was that$T_g$ value of H-H copolymer was higher than that of the corresponding H-T structure. Decomposition temperature of the H-H copolymer was lower than that of the H-T copolymer. All the H-H and H-T copolymers were soluble in common solvents.

1H NMR Study of Aziridine Derivatives Coordinated to the Paramagnetic Undecatungstocobalto(II)silicate and -nickelo(II)silicate Anions

  • 박석민;서현수
    • Bulletin of the Korean Chemical Society
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    • v.18 no.9
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    • pp.1002-1006
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    • 1997
  • 1H NMR spectra of D2O solutions containing 2,2-dimethylaziridine (1) or 2-methylaziridine (2) and [SiW11COⅡO39]6- (SiW11Co) or [SiW11NiⅡO39]6- (SiW11Ni) exhibit separate signals for the free ligand and the complex, indicating that the ligand exchange is slow on the NMR time scale. Identified are two linkage isomers with the methyl group of 2 at trans or cis position with respect to the metal. The isotropic shifts of 1 and 2 coordinated to SiW11Ni originate mainly from the contact shifts, and they agree reasonably with the relative values reported for similar ligands coordinated to bis(2,4-pentanedionato)nickel(Ⅱ). The isotropic shifts for the SiW11Co complexes were separated into contact and pseudocontact contributions. The pseudocontact shifts show that (χ∥-χ⊥) is positive, while that for the SiW11Co complexes of pyridine derivatives is negative. This result indicates that the ordering of dxy and dxz, dyz orbitals in SiW11Co complexes can be reversed by ligands.

Studies on the Oxidative Addition Reactions of 1-Bromosilatranes to $SnBr_2$ (1-브로모실라트란의 $SnBr_2$ 에 대한 산화성 첨가반응 연구)

  • Kim, Myeong Un;Eo, Dong Seon;Sin, Ho Cheol;Kim, Jin Gwon;Do, Young Gyu
    • Journal of the Korean Chemical Society
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    • v.38 no.3
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    • pp.241-245
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    • 1994
  • The oxidative addition reaction has been employed to synthesize heteropolynuclear compounds containing Si-M bonding interaction between the silicon atom of silatrane, pentacoordinate silicon derivative with transannular Si-N dative bond, and the main group element. The reaction of $SnBr_2 with 1-bromosilatrane(1a) in acetonitrile gives the mixture of yellow(2a) and white(2b) solids which were isolated and charaterized by ^1H-NMR, ^{29}Si-NMR, ^{119}Sn-NMR and Mass spectroscopy. The yellow compound was characterized as 1-tribromotinsilatrane which had Si-Sn bonding interaction. The reaction of SnBr2 with 1-bromo-3,7,10-trimethylsilatrane(1b) in methanol gives the Sn(Ⅳ) complex, N[CH_2CH(CH_3)O]_3SiSnBr_3(CH_3OH)_2(3),$ which was characterized by various means.

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토양균에서 항생물질 및 효소억제제의 분리와 구조 연구

  • 구양모;이윤영;김경자;최응칠;김범태;주정호;이창훈
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1994.04a
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    • pp.179-179
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    • 1994
  • 새로운 항생물질을 개발하기 위하여 토양으로부터 분리한 균주를 액체 및 고체배지에서 배양하여 여러 검정균에 대하여 종이디스크법으로 항균효력을 조사하였다. 그 결과 (+), G(-), fungi 등에 강한 항균 효력을 보인 토양균 SNUS 8810-43과 Mycobacterium, fungi에 항균력을 보인 토양균 SNUS 8810-129를 선택하여 각각의 배양액에서 항생물질을 분리하고, 분리한 항생물질의 구조를 규명하고자 하였다. 토양균 SNUS 8810-43의 배양액으로부터 항생물질을 분리하기 위하여 양이온 교환 수지 관 크로마토그래피와 셀룰로오스 관 크로마토그래피를 수행하여 시료 JJH-II-46-43을 얻었다. 시료 JJH-II-46-43의 IR, $^1$H-NMR, $^{13}$C-NMR, $^1$H-$^1$H COSY, $^1$H-$^{13}$C COSY, FAB-MS 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질의 구조가 N-methylstreptothricin과 동일하다는 것을 확인하였다. Mycobacterium smegmatis에 강한 활성을 나타내는 물질을 토양균 SNUS 8810-129로 부터 분리하였다. 토양균 SNUS 8810-129를 배양한 V-8 아가판을 메탄올로 추출하여 이를 실리카겔 관 크로마토그래피와 preparative TLC로 시료 LCH-IV-17B, LCH-III-387을 얻었다. 시료LCH-IV-l7B, LCH-III-387의 $^1$H-NMR, $^{13}$C-NMR, FAB-MS, CI-MS, IR등의 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질이 glycolipid계 항생물질이라는 것을 알았다. $^{13}$C-NMR 상의 자료와 화학적인 방법으로 구성당을 조사한 결과 이 항생물질을 이루고있는 당은 rhamnose 임을 알았다. 또 이 항생물질을 구성하는 지방산은 화학적인 방법과 MS 스펙트럼, $^{13}$C-NMR 스펙트럼으로부터 hydroxydecanoic acid인 것으로 확인되었다. 항생물질 LCH-III-387와 항생물질 LCH-IV-l7B는 각각 rhamnose를 1, 2개 포함하고 있는 것으로 확인되었다. 그리고 동일한 탄소수의 지방산을 가지고 있는 것으로 생각되었다. 이들 항생물질을 이루는 구성당과 지방산간의 정확한 연결및 구조, 생리활성에 관한 연구는 계속 수행중에 있다.

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Phenolic Compounds from Bark of Juglans mandshurica (가래나무 수피의 페놀성 화합물)

  • Kim, Jin-Kyu;Si, Chuan-Ling;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.34 no.6
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    • pp.51-60
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    • 2006
  • Juglans mandshurica barks were collected, extracted with acetone-$H_2O$ (7:3, v/v), fractionated with n -hexane, $CH_2Cl_2$, and EtOAc, and freeze dried to give some dark brown powder. The EtOA cand $H_2O$ soluble fractions were chromatographe d on a Sephadex LH-20 column using $H_2O$-MeOH and EtOH-hexane mixture as eluents. Spectrometric analysis such as NMR and MS, including TLC,were performed to characterize the structures of the isolated compounds. From the EtOAc and $H_2O$ soluble fractions, three flavanols (1~3), three flavonols (4~6) and five flavonol glycosides (7~11) were isolated and elucidated.

($^{11}$B NMR study of vortex dynamics in LuNi$_2$B$_2$C

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Cho, B.K.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.107-110
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    • 2000
  • ($^{11}$B NMR measurements have been performed on single crystals of LuNi$_2$B$_2$C superconductor to investigate vortex lattice structures and dynamical behavior. The spectrum in the superconducting state is significantly broadened by local field inhomogeneity due to the vortex lattice and the peak point of the spectrum shifts toward low magnetic field due to the imperfect field penetration. The linewidth of the spectrum reflecting local field variation is much smaller than expected for conventional vortex lattices and shows peculiar increase at low temperature. Furthermore, the transverse relaxation rate, 1/T$_2$, probing the slow motion of vortices, exhibits a single peak as temperature decreases. These prominent results highlight significant fluctuation of vortices even for this low T$_c$, and nearly isotropic 3D superconductor.

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Synthesis and Characterization of Palladium (IV) Complexes with Guanine, Adenine, and Uracil Base (Guanine, Adenine 및 Uracil 염기를 갖는 팔라듐 (IV) 착물의 합성과 그 성질)

  • Oh Sang Oh;Chung Duck Young;Kim Hee Seon
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.679-684
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    • 1992
  • New Pd(IV) complexes have been prepared through the reactions of $trans-[Pd(en)_2Cl_2](ClO_4)_2 $(en = ethylenediamine) with Guanine, Adenine, or Uracil anion as purine and pyrimidine base. We identified the ratio of central metal versus ligands by $C{\cdot}H{\cdot}N$ elemental analysis and proposed the coordinating site of the base by infrared spectrum, $^1H-NMR,\; and\; ^{13}C$-NMR spectrum. Guanine or Adenine ligand coordinated at N7 site and an en ligand exchanged for $ClO_4^-$ counter ions of the starting material . As these results, the complexes showed the formula $[Pd(en)L_2(ClO_4)_2](ClO_4)_2{\cdot}(en)$, (L = Guanine, Adenine). But in the Uracil complex no exchange of the en ligand and $ClO_4^-$ occured and Uracil anion preferred the N1 to N3 as coordinating site, the complex $[Pd(en)_2(Urac)_2](ClO_4)_2(Urac = Uracil anion).$

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Identification of NMR Data for ginsenoside Rg1 (Ginsenoside Rg1의 NMR 데이터 동정)

  • Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Park, Hee-Jeong;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.32 no.4
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    • pp.291-299
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    • 2008
  • The fresh ginseng roots were extracted in aqueous methanol (MeOH), and the obtained extracts were partitioned using ethyl acetate (EtOA), n-butanol (n-BuOH), and water, successively. The repeated silica gel column chromatography for n-BuOH fraction afforded a purified ginsenoside $Rg_1$. The physico-chemical, spectroscopic and chromatographic data of ginsenoside $Rg_1$, such as crystallization characteristics, melting point, specific rotation, infrared spectrometry (IR) data, fast atom bombardment/mass spectrometry (FAB/MS) data, nuclear magnetic resonance (NMR) data, retention factor (Rf) in thin layer chromatography (TLC) experiment, and retention time (r.t.) in HPLC analysis, were measured and compared with those reported in literatures. Especially, the previous literatures reported different data for ginsenoside $Rg_1$ in the $^{1}H-$ and $^{13}C$-NMR experiments. This paper gives the exactly assigned NMR data through 2D-NMR experiments, such as $^{1}H-^{1}H$ correlation spectroscopy (COSY), hetero nuclear single quantum correlation (HSQC), and hetero nuclear multiple bond connectivity (HMBC).

Purification and Characterization of the Regulatory Substance of Furfural Biodegradation in Pseudomonas fluorescens (Pseudomonas fluorescens에 의한 Furfural의 분해대사 조절물질에 관하여)

  • 이병웅;유병설;이계준;하영칠
    • Korean Journal of Microbiology
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    • v.23 no.4
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    • pp.241-247
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    • 1985
  • The objectives of this study were to isolate and identify ninhydrin positive substande(s) produced in the culture broth of Pseudomonas fluorescens. It was found that the NPS could stimulate bioconversion of furfural into furoic acid. In order to isolate the NPS from the culture broth, cell free filtrate was subjected to ion-exchange chromatography, gel-permeation and finally to cellulose column chromatography. The purified NPS was white amorphous power and very soluble in water, slightly soluble in methanol and very insoluble in organic solvents. UV, and IR absorption spectra. $^H$ and $^{13}C-NMR$ were measured in order to identify the chemical structure of the NPS.

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