• Title/Summary/Keyword: NMR and Mass Spectra

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Synthesis and Characterization of Group 13 Compounds of 2-Acetylpyridine Thiosemicarbazone. Single-Crystal Structure of $(iC_4H_9)-2Al(NC_5H_4C(CH_3)$NNC(S)NHPh)

  • 강영진;강상옥;고재정;손정인
    • Bulletin of the Korean Chemical Society
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    • v.20 no.1
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    • pp.65-68
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    • 1999
  • Novel mononuclear group 13 metal complexes with the formula (R2M){NC5H4C(CH3)NNC(S)NH(C6H5)} (M=Al, R=iC4H9 (1); M=Ga, R=iC4H9 (2); M=Al, R=CH2SiMe3 (3); M=Ga, R=CH2SiMe3 (4)) result when 2-acetyl pyridine 4-phenyl-thiosemicarbazone ligand is mixed with trialkyl aluminum or trialkylgallium. These compounds 1-4 are characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and singlecrystal X-ray diffraction. X-ray single-crystal diffraction analysis reveals that 1 is mononuclear metal compound with coordination number of 5 and N, N, S-coordination mode.

Studies on the Morphology and the Chemotaxonomy of Citrus Plants Native to Je Ju Island and on its Application (II) -On the Chemical Components of Citrus platymamma Hort. ex Tanaka- (제주도 재래감귤의 식물학적 특성과 이용에 관한 연구 (II) -병귤(甁橘)의 성분연구-)

  • Kim, Chang-Min;Huh, In-Ok;Han, Dae-Suk
    • Korean Journal of Pharmacognosy
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    • v.10 no.2
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    • pp.85-87
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    • 1979
  • 제주도(濟州道) 재래감귤인 병귤(甁橘) Citrus platymamma $H_{ORT}$. ex $T_{ANAKA}$의 엽(葉), 과피(果皮), 수피(樹皮)의 클로로포롬 가용부(可容部)에서 무색침장정(無色針狀晶), $C_{10}H_{10}O_{4}$, mp $139{\sim}140^{\circ}c$을 단리(單利)하고 이화학적(理化學的) 성상(性狀)및 UV, IR, NMR, Mass spectra를 이용하여 그 화학구조(化學構造)를 구명(究明)한바 1,4-benzenedicar-boxylic acid dimethyl ester이었다. 또 과피(果皮)의 수용부(水溶部)에서 단리(單利)한 2개의 flavonoid 배당체(配糖體)는 그 이화학적(理化學的)인 성상(性狀) 및 IR-spectrum으로 보아 naringin hesperidin이었다.

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The Chemical Constituents of Bezoar Bovis (우황 (Bezoar Bovis)의 성분연구)

  • In Kyu Kim;Sun Ku Park;Hyun Cheol Oh;Kyu Wan Kim
    • Journal of the Korean Chemical Society
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    • v.35 no.3
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    • pp.249-252
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    • 1991
  • Two new metabolites have been characterized from the methylene chloride extracts of Bezoar Bovis, a well known oriental drug : 8-octadecenoic methyl ester and cholesta-3,5-diene. Their structures were deduced from $^1$H-NMR and GC-mass spectra.

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Physicochemical Characterization and NMR Assignments of Ginsenosides Rb1, Rb2, Rc, and Rd Isolated from Panax ginseng

  • Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Park, Hee-Jung;Lee, Dae-Young;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.34 no.2
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    • pp.113-121
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    • 2010
  • The fresh ginseng roots were extracted with aqueous methanol, and the obtained extracts were partitioned using ethyl acetate, n-butanol, and water, successively. The repeated silica gel and octadecyl silica gel column chromatogaraphy for n-butanol fraction afforded four diol ginseng saponins, ginsenosides $Rb_1$, $Rb_2$, $R_c$, and Rd. The physicochemical, spectroscopic, and chromatographic characteristics of these ginsenosides were measured and compared with those reported in the literature. Some of the peak assignments in previously published $^1H$- and $^{13}C$-nuclear magnetic resonance (NMR) spectra were inaccurate. This study employed two-dimensional NMR experiments, including $^1H-^1H$ correlation spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond connectivity, to determine exact peak assignments.

Synthetic, Characterization, Biological, Electrical and Catalytic Studies of Some Transition Metal Complexes of Unsymmetrical Quadridentate Schiff Base Ligand

  • Maldhure, A. K.;Pethe, G. B.;Yaul, A. R.;Aswar, A. S.
    • Journal of the Korean Chemical Society
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    • v.59 no.3
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    • pp.215-224
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    • 2015
  • Unsymmetrical tetradentate Schiff base N-(2-hydroxy-5-methylacetophenone)-N'-(2-hydroxy acetophenone) ethylene diamine (H2L) and its complexes with Cr(III), Mn(II), Fe(III), Co(II), Ni(II) and Cu(II) have been synthesized and characterized by elemental analyses, magnetic susceptibility measurements, IR, electronic spectra and thermogravimetric analyses. 1H, 13C-NMR and FAB Mass spectra of ligand clearly indicate the presence of OH and azomethine groups. Elemental analyses of the complexes indicate that the metal to ligand ratio is 1:1 in all complexes. Infrared spectra of complexes indicate a dibasic quadridentate nature of the ligand and its coordination to metal ions through phenolic oxygen and azomethine nitrogen atoms. The thermal behavior of these complexes showed the loss of lattice water in the first step followed by decomposition of the ligand in subsequent steps. The thermal data have also been analyzed for the kinetic parameters by using Horowitz-Metzger method. The dependence of the electrical conductivity on the temperature has been studied over the temperature range 313-403 K and the complexes are found to show semiconducting behavior. XRD and SEM images of some representative complexes have been recorded. The antimicrobial activity of the ligand and its complexes has been screened against various microorganisms and all of them were found to be active against the test organisms. The Fe(III) and Ni(II) complex have been tested for the catalytic oxidation of styrene.

Synthesis and Spectral Properties of 1,2-Bispyrazyl Ethylene (1,2-비스피라질 에틸렌의 합성과 분광학적 성질에 대한 연구)

  • Shim Sang Chul;Lee Dong Soo;Chae, Jeong Seok;Song Pili Soon
    • Journal of the Korean Chemical Society
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    • v.20 no.5
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    • pp.398-405
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    • 1976
  • A new compound, 1,2-bispyrazyl ethylene,is synthesized starting from pyrazine carboxylic acid and methyl pyrazine. The compound is characterized utilizing UV-VIS, IR, NMR and mass spectra along with elemental analysis. Spectroscopic properties are studied from UV-VIS and fluorescence spectra. From unusual salt effects on fluorescence spectra, it is believed that $(n,\;{\pi}^*)$ state has about the same energy as $({\pi},\;{\pi}^*)$ state. The compound fluoresces from $({\pi},\;{\pi}^*)$ state with the quantum yield of 0.025 at $77^{\circ}K$ compared to near unity for stilbene at the same temperature indicating the efficient intersystem crossing to triplet state, because of strong $(n,\;{\pi}^*)$ and $({\pi},\;{\pi}^*)$ mixing in the lowest excited state.

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Performance of a Novel Sulfonate Flame Retardant Based on Adamantane for Polycarbonate (아드만탄 기반의 새로운 설포네이트 폴리카보네이트 난연제 성능 연구)

  • Guo, Jianwei;Wang, Yueqin;Feng, Lijuan;Zhong, Xing;Yang, Chufen;Liu, Sa;Cui, Yingde
    • Polymer(Korea)
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    • v.37 no.4
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    • pp.437-441
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    • 2013
  • A novel sulfonate flame retardant, 1,3,5,7-tetrakis(phenyl-4-sodium sulfonate)adamantane (FR-A), was successfully synthesized from 1-bromoadamantane in sequential four-step reactions involving Fiedel-Crafts phenylation, sulphonation, hydrolysis, and neutralization. The success of synthesis was confirmed by FTIR spectra, $^1H$ NMR spectra, elemental analyses and mass spectra. The effect of FR-A on the flame retardacy of polycarbonate (PC) has been studied. Limiting oxygen index (LOI) and thermogravimetric analysis (TGA) showed that this novel sulfonate flame retardant had effective flame retardancy on polycarbonate (PC). With a small amount (0.08 wt%) of FR-A, the flame retardancy of PC was improved obviously, which got to UL 94 V-0 rating. TGA and DTA curves demonstrated that the additive raised the degradation rate of PC by promoting the quick formation of an insulating carbon layer on the surface, and confirmed that the flame retardant mechanism of PC/FR-A system was similar to potassium diphenylsulfone sulfonate (KSS).

Isolation and Identification of α-Glucosidase Inhibitory Compounds, Hyperoside, and Isoquercetin from Eleutherococcus senticosus Leaves (가시오갈피(Eleutherococcus senticosus) 잎으로부터 α-Glucosidase의 저해 활성 물질, Hyperoside와 Isoquercetin의 분리 및 구조·동정)

  • Lee, Ki Yeon;Hong, Soo Young;Jeong, Hye Jeong;Lee, Jae Hyoung;Lim, Sang Hyun;Heo, Nam-Kee;Kim, Songmun;Kim, Hee-Yeon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.12
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    • pp.1858-1864
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    • 2014
  • In the present investigation, the anti-diabetic potential of 80% ethanol extract of Eleutherococcus senticosus leaves (EEES) was examined based on ${\alpha}$-glucosidase inhibitory activities. EEES was sequentially fractionated with n-hexane, chloroform, ethyl acetate (EtAOc), n-butanol, and $H_2O$. Of the various fractions, EtAOc fraction effectively inhibited ${\alpha}$-glucosidase activity by 68.05%. Therefore, EtAOc fraction was selected for further isolation and identification studies. EtAOc fraction was separated by medium pressure liquid chromatography with silica and ODS gel to yield eight fractions (EAA~EAH). Based on the results of ${\alpha}$-glucosidase inhibitory activity, EAH fraction was re-chromatographed to yielded four more fractions (EAHA~EAHD). Of these, EAHC fraction showed higher ${\alpha}$-glucosidase inhibitory activity of 93.60%. EAHC fraction was re-chromatographed and yielded EAHCA and EAHCB fractions. Further, identification and chemical structures of these two fractions were analyzed using $^1H$-NMR, $^{13}C$-NMR, and mass spectra data. Based on the results of the spectral data, the isolated compounds were identified as hyperoside and isoquercetin. Results of the present study indicate that the isolated compounds, hyperoside, and isoquercetin from leaves of E. senticosus could be used for the development of new anti-diabetic drugs.

Preparation and Properties of Phytosphingosine Ascorbate with Retaining Skin Development Effects (피부 활성을 갖는 Phytosphingosine Ascorbate의 합성)

  • Min, Seok-Kee;Jin, Yong-Hoon;Park, Woo-Jung;Eom, Sang-Yong;Kim, Jong-Heon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.30 no.2
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    • pp.167-172
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    • 2004
  • In the human skin, vitamin C (L -ascorbic acid) that is well known as the activated materials has effects that is skin anti-aging and wrinkle repair by giving impetus to collagen biosynthesis and anti-oxidation, and that is the sun screen, a wound recovering, inhibition melanogenesis and so on. In spite of its effects, vitamin C has the defects of the skin stimulation and easily oxidized instability by water, air, heat and light. For solving their matters, many investigation is advanced and its results are synthesized the various vitamin C derivatives. And yet they have not solved the unstable property of vitamin C and were still insufficient for the comparing with the effect of the pure vitamin C itself. In this study, in order to prepare vitamin C derivative of being improved the stability and to apply vitamin C effect in the skin, we prepared new vitamin C derivative, phytosphingosine ascorbate, by using phytosphingosine, one of sphingolipids, which have a distinguished skin affinity. Phytosphingosine ascorbate can be prepared as the ionic bond between amine group (-NH$_2$) of phytosphingosine and hydroxy group (-OH) of vitamin C by way of the relatively simple reaction. So the structure and properties of the synthesized phytosphingosine ascorbate was confirmed the use of elemental analysis (C 58.3 : H 9.3 : N 2.8 : O 29.5), MALDI TOF-MS (Mw=492.58), Ultraviolet spectra (268.5nm), lH NMR, FT-IR spectra, thermal analysis (m.p=l54$^{\circ}C$), HPLC and so on. And we could confirm the anti-bacterial and anti-oxidation effects. Based on these results, we could confirm to prepare a new material that was expected of both effects of vitamin C and phytosphingosine and that is improved properties of vitamin C.

Polyacetylene Compounds from Panax ginseng C.A. Meyer (인삼의 Polyacetylene 화합물)

  • Shim Sang Chul;Chang Suk-Ku
    • Proceedings of the Ginseng society Conference
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    • 1988.08a
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    • pp.122-128
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    • 1988
  • Several major polyacetylene compounds were isolated from the petroleum-ether fraction of fresh Korean ginseng roots through solvent fractionation. partition and silica gel column chromatography. Further separation of acetylenic compounds was accomplished by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The preparative separation for the various spectral measurements was carried out by low pressure preparative liquid chromatography. The chemical structure of these polyacetylenes separated was determined by UV. IR/FTIR. $^{1}H$ NMR. mass spectral and elemental analysis. These are identified to be heptadeca-1-en-4.6-diyn-3.9.l0.-triol [1] heptadeca-1.9-dien-4.6-diyn-3-ol. heptadeca-1.8-dien-4.6-diyn-3.10-diol and the 4th was denatured polyacetylene. heptadeca-1.4-dien-6.8-diyn-3.10-diol. Two different p-substituted benzoates of panaxynol were synthesized for the determination of exciton chirality. The circular dichroism spectra in the UV region show that panaxynol p-bromobenzoate and p-dimethyl-aminobenzoate constitute negative exciton chirality [2]. Isolated major polyacetylene compounds were irradiated in aerated solution with 300 nm UV light to obtain the oxidized product at the allylic alcohol center to corresponding carbonyl compounds such as heptadeca-1-en-4.6-diyn-9.10-diol-3-one and heptadeca-1.9-dien-4.6-diyn-3-one. These photooxidation compounds have en-on-diyne chromophore and undergo nucleophilic addition reaction with methanol to yield ${\beta}-methoxy$ carbonyl compounds such as heptadeca-9-en-4.6-diyn-1-methoxy-3-one and heptadeca-4.6-diyn-1-methoxy-9.10-diol-3-one.

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