• Title/Summary/Keyword: H-NMR spectroscopy

Search Result 628, Processing Time 0.029 seconds

Synthesis and the Absolute Configurations of Isoflavanone Enantiomers

  • Won, Dong-Ho;Shin, Bok-Kyu;Han, Jae-Hong
    • Journal of Applied Biological Chemistry
    • /
    • v.51 no.1
    • /
    • pp.17-19
    • /
    • 2008
  • Isoflavanone has been synthesized from the reduction of isoflavone in nearly quantitative yield. Isoflavone with seven equivalents of ammonium formate in the presence of Pd/C in ethanol under $N_2$ atmosphere exclusively produced the two-electron reduced product in two hours. It was characterized by various spectroscopic methods, including UV-VIS, EI-MS, $^1H$-NMR, $^{13}C$-NMR and $^1H$, $^1H$-COSY. The racemic mixture was separated by Sumi-Chiral column chromatography and the absolute configurations of the enantiomers were characterized by circular dichroism spectroscopy.

The Synthesis and Characterization of Some Novel Thioethers: Thio-Subsituted [3]Cumulenes, -1-Buten-3-ynes and Buta-1,3-dienes

  • Ibis, Cemil;Sahin, Aysecik
    • Bulletin of the Korean Chemical Society
    • /
    • v.31 no.8
    • /
    • pp.2255-2260
    • /
    • 2010
  • In this study, some novel thiosubstituted butenyne (3a-d, 7b, 15b), butadiene (4a-b, 4d, 5a, 5c, 6b, 8e, 9c, 10b, 16b, 18e) and [3]cumulene (11a-b with isomer 3a-b, 12a with isomer 13a, 14b, 17e) compounds were synthesized from the reaction of 2H-pentachloro-1,3-butadiene with thiols. The new compounds were characterized by elemental analysis, mass spectrometry, UV-vis, IR, 1H NMR, NMR ($^{13}C$ or APT) spectroscopy.

Intramolecualr cyclization of a dipyrromethane by an electrophilic aromatic substitution reaction producing a new chiral compound

  • Kim, Seung Hyun;Kim, Sung Kuk
    • Journal of the Korean Magnetic Resonance Society
    • /
    • v.22 no.4
    • /
    • pp.115-118
    • /
    • 2018
  • Dipyrromethane 2 functionalized with 3-chloropropyl group on the meso carbon undergoes an unusual intramolecular electrophilic aromatic substitution reaction in the presence of $NaN_3$ instead of a simple nucleophilic substitution reaction. As a result, a new chiral dipyrromethane 1 was synthesized. In this reaction, the ${\beta}$-carbon of the pyrrole ring functions as a nucleophile while the carbon next to the chlorine atom acts as an electrophile. Interestingly, this reaction progresses even in the absence of an acid catalyst. Compound 1 was fully characterized by $^1H-^1H$ and $^1H-^{13}C$ COSY NMR spectroscopic analyses and the high resolution EI mass spectrometry.

Precise Control of Thermoresponsive Properties of Polymers with Hydroxy Groups in the Side Chains (곁가지에 다양한 길이의 알코올 그룹을 지닌 고분자들의 저임계 용액온도 민감성 제어)

  • Lee, Hyung-Il
    • Polymer(Korea)
    • /
    • v.39 no.1
    • /
    • pp.165-168
    • /
    • 2015
  • Thermoresponsive polymers were successfully synthesized by a combination of atom transfer radical polymerization (ATRP) and Cu(I)-catalyzed 1,3-dipolar cycloaddition of azide and alkynes (click chemistry). Poly(2-hydroxyethyl methacrylate) (PHEMA) was synthesized by ATRP, followed by introduction of alkyne groups using pentynoic acid, leading to HEMA-alkyne. Homopolymers having secondary amine groups, tertiary amines with hydroxyethyl and hydroxypropyl groups were synthesized by adding 2-azido-N-ethyl-ethanamine, 2-[(2-azidoethyl)amino]ethanol, and 2-[(2-azidoethyl)amino]propanol, respectively, to the PHEMA-alkyne backbone using click chemistry. Molecular weight (MW), molecular weight distribution (MWD), and click reaction efficiency were determined by gel permeation chromatography (GPC) and $^1H$ NMR spectroscopy. The transmission spectra of the 1.0 wt% aqueous solutions of the resulting polymers at 650 nm were measured as a function of temperature. Results showed that the lower critical solution temperature (LCST) could be easily controlled by the length of the hydroxyalkyl groups.

Synthesis of Organic Silicon Compounds from Siliceous Mudstone (규질이암으로부터 실리콘 유기화합물 합성)

  • Kim, Byoung-Gyu;Jang, Hee-Dong;Kim, Jong-Seok
    • Journal of the Mineralogical Society of Korea
    • /
    • v.20 no.3
    • /
    • pp.155-163
    • /
    • 2007
  • A novel route to the synthesis of tetramethoxysilane and other silicon alkoxides is described using siliceous mudstone as the raw material. The reaction of amorphous silica with triethanol-amine is enhanced by using an alkali metal hydroxide catalyst to form a range of triethanol-amnine-substituted silatrane species. These can undergo alkoxide exchange in acidic alcohols to form alkoxysilatranes, tetraalkoxysilanes, hexaalkoxydisiloxanes and higher siloxanes. Products were identified by FT-IR spectroscopy, XRD, SEM, 1H and 13C NMR spectroscopy, or gas chromatography.

A Study on Synthesis and Characterization of Dinitrosylmolybdenum Complexes (디니트로실 몰리브덴 착물의 합성과 특성에 관한 연구)

  • Doh, Kiel Myung;Kim, Ill Chool;Choi, Bo Yong
    • Journal of the Korean Chemical Society
    • /
    • v.39 no.3
    • /
    • pp.191-197
    • /
    • 1995
  • The reactions of [${Mo(NO)_2Cl_2}_n$] with unidentate ligands in $CH_2Cl_2$ solvent afforded monomeric complexes [$Mo(NO)_2L_2Cl_2$]. $[Mo(NO)_2L_4](ClO_4)_2$ was obtained by reaction of unidentate with $[Mo(NO)_2L_2Cl_2]$ in aceton solvent. 4-Dimethylaminopyridine(dmap), pyridine(py), and isoquinoline(isoq) were used as coordinating ligands. These dinitrosylmolybdenum complexes are prepared and characterized by elemental analysis, $^1H$ NMR, infrared, and UV-Visible spectroscopy. The infrared spectra indicate that the NO groups occupy cis-positions of the octahedral.

  • PDF

The Action Mode of $\beta$-glucosidase Purified from Trichoderma koningii (Trichoderma koningii에서 분리한 $\beta$-glucosidase의 작용양상)

  • 정춘수;최지영;이헌주;맹필재;한인섭;강사욱;하영칠
    • Korean Journal of Microbiology
    • /
    • v.36 no.1
    • /
    • pp.8-13
    • /
    • 2000
  • We have examined the mode of transglycosylation, catalyzed by an extracellular $\beta$-glucosidase purified from Trichoderma koningii ATCC 26113, using cellobiose, sophorose, laminaribiose and gentiobiose as substrates. The dimers separated from the reaction mixture by HPLC were analyzed by $^(1)H$-NMR spectroscopy. When cellobiose was subjected to the action of the $\beta$-glucosidase, the products included laminaribiose, sophorose and gentiobiose. When laminaribiose, sophorose or gentiobiose was used as a substrate, the $\beta$-glucosidase accumulated transglycosylation products possessing different types of $\beta$-glycosidic linkages from the original one. The amount of dimers accumulated as reaction proceeded seemed to be dependent on the velocity of hydrolysis but not on that of formation.

  • PDF

A Study on the Preparation of new Functionalized Aminosilanes as a Promising Coupling Agent(I) (결합제로서 가능성 있는 새로운 작용기를 갖는 Aminosilane 제조에 관한 연구(I))

  • 한정식
    • Journal of the Korean Society of Propulsion Engineers
    • /
    • v.2 no.3
    • /
    • pp.47-53
    • /
    • 1998
  • Using Michael Reaction, commercially available 3-aminopropyltrimethoxysilane and N-[3-(trimethoxysilyl)propuyl]ethylenediamine were reacted with various Michael acceptors, ethyl acrylate, acrylonitrile, acrylamide, 2-cyanoethyl acrylate, 2-hydroxyethyl acrylate and 3-(trimethoxysilyl)propylmethacrylate, to the new aminosilanes. All compounds which are [3-(N-2-carboethoxyethyl)aminopropyl]triethoxysilane, [3-(N-2-cyanoethyl)aminopropyl]triethoxysilane, [3-(N-di-2-car-boethoxyethyl)aminopropyl]triethoxysilane, [3-N-di-cyanoethyl) aminopropyl]triethoxysilane, [3-(N-2-cyanoethoxypropionyl)aminopropyl]triethoxysilane, [3-(N-di-2-cyanoethoxypropionyl)aminopropyl]triethoxysilane, [3-(N-di-2-hydroxyethoxy propionyl)aminopropyl]triethoxysilane, [3-(N-2-amidoethyl)aminopropyl]triethoxysil-ane,{3-[N-(N-di-2-cyanoethyl)ethyl]aminopropyl}triethoxysilane and {3-[N-(3-trimethoxysilylpropyl)-2-methylpropionyl]aminopropyl}triethoxysilane were succes-sfully prepared in 35-70% yields and which were identified with $^1{H}$-NMR and FT-IR spectroscopy.

  • PDF

Spectroscopic Characterization and Seasonal Distribution of Aquatic Humic Substances Isolated from Han River Water (한강원수로부터 분리된 수중휴믹물질의 계절적 분포와 분광학적 특성분석)

  • Kim, Hyun-Chul;Lee, Seock-Heon;Kim, Kyung-Ju;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.29 no.5
    • /
    • pp.540-547
    • /
    • 2007
  • Humic substances(HS) from Han River water was physic-chemically isolated by fractionational methods to investigate the seasonal distribution and to characterize the properties compared with intrinsic humic materials. Various HS samples were analyzed by element, Fourier transform infrared(FT-IR), proton nuclear magnetic resonance$(^1H-NMR)$ and fluorescence analyzers. The portion of HS from Han River water(HRHS) was 47.0% on the average, however it appeared that rainfall event brought about higher fraction of HS in Han River water by the periodic investigation. Aromaticity and humification degree of the HRHS were relatively lower than those of intrinsic humic materials originated from decomposing vegetation. FT-IR, $^1H-NMR$ and fluorescence spectroscopy showed the distinct differences between HRHS and intrinsic humic materials. Commercial humic materials could not represent structural and functional characteristics of local HS. The fluorescence spectroscopy, a relatively simple measurement, was found most useful tool to estimate humification degree for humic materials from particular sources.

Complete $^1H$-NMR and $^{13}C$-NMR spectral analysis of the pairs of 20(S) and 20(R) ginsenosides

  • Yang, Heejung;Kim, Jeom Yong;Kim, Sun Ok;Yoo, Young Hyo;Sung, Sang Hyun
    • Journal of Ginseng Research
    • /
    • v.38 no.3
    • /
    • pp.194-202
    • /
    • 2014
  • Background: Ginsenosides, the major ingredients of Panax ginseng, have been studied for many decades in Asian countries as a result of their wide range of pharmacological properties. The less polar ginsenosides, with one or two sugar residues, are not present in nature and are produced during manufacturing processes by methods such as heating, steaming, acid hydrolysis, and enzyme reactions. $^1H$-NMR and $^{13}C$-NMR spectroscopic data for the identification of the less polar ginsenosides are often unavailable or incomplete. Methods: We isolated 21 compounds, including 10 pairs of 20(S) and 20(R) less polar ginsenosides (1-20), and an oleanane-type triterpene (21) from a processed ginseng preparation and obtained complete $^1H$-NMR and $^{13}C$-NMR spectroscopic data for the following compounds, referred to as compounds 1-21 for rapid identification: 20(S)-ginsenosides Rh2 (1), 20(R)-Rh2 (2), 20(S)-Rg3 (3), 20(R)-Rg3 (4), 6'-O-acetyl-20(S)-Rh2 [20(S)-AcetylRh2] (5), 20(R)-AcetylRh2 (6), 25-hydroxy-20(S)-Rh2 (7), 25-hydroxy-20(S)-Rh2 (8), 20(S)-Rh1 (9), 20(R)-Rh1 (10), 20(S)-Rg2 (11), 20(R)-Rg2 (12), 25-hydroxy-20(S)-Rh1 (13), 25-hydroxy-20(R)-Rh1 (14), 20(S)-AcetylRg2 (15), 20(R)-AcetylRg2 (16), Rh4 (17), Rg5 (18), Rk1 (19), 25-hydroxy-Rh4 (20), and oleanolic acid 28-O-b-D-glucopyranoside (21).