• Title/Summary/Keyword: 1H-NMR spectroscopy

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Effect of Length of Alkyl Group on Thermal-Liquid Crystalline Properties of Cholesteryl 4-n-Alkoxybenzoate (알킬기의 길이가 콜레스테릴 4-n-알콕시벤조에이트의 열적-액정 특성에 미치는 영향)

  • Yoon, Doo-Soo;Bang, Moon-Soo
    • 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.

Sequence Distribution and Thermal Properties of Poly(butylene succinate-co-butylene terephthalate) Copolyesters (Poly(butylene succinate-co-butylene terephthalate) 공중합물의 미세구조와 열적 성질)

  • Park, Sang Soon;Jeong, Jae Ho;Kim, Tae Jeong;Kim, Dae Jin;Im, Seung Soon
    • Journal of the Korean Chemical Society
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    • v.40 no.1
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    • pp.87-95
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    • 1996
  • The binary random copolyesters of poly(butylene succinate-co-butylene terephthalate) (PBS/PBT) were synthesized and their sequence distributions were investigated over the entire range for PBS/PBT copolyester compositions by 1H NMR spectroscopy. The melting point (Tm) of these copolyesters were depressed gradually with the increase of dimethyl terephthalate (DMT) mol% in composition and appeared an eutetic behaviour which appears a minimum at ST3 (DMT 65.8 mol%). The melting behaviour of PBS/PBT copolyester was not directly depended on molar fraction (Xa) but on only the sequence propagation probability (P) which occurs in triad fraction. It also can be seen that when the succinate units (or terephthalate units) were abundant enough, PBS/PBT Copolymers formed only PBS (or PBT) crystal with complete rejection of the terephthalate units (or succinate units).

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Synthesis and Characteristics of Photo-crosslinkable Hydrogel for Microbial Immobilization (미생물 고정화를 위한 광경화성 하이드로겔의 합성과 특성)

  • Kim, Cho Woong;Lee, Jung Bock;Kim, Du Hyun;Hwang, Jung Min;Cho, Chong Su;Choi, Young Hoon;Chung, Dae-Won
    • Applied Chemistry for Engineering
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    • v.10 no.6
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    • pp.852-856
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    • 1999
  • The objective of this study was to prepare hydrogel beads which were useful microbial immobilization to remove nitrogen and phosphorous in the industrial wastewater. Two different polyols(PEG, PTMG) terminated with photo-crosslinkable methacrylate groups were synthesized. Structures of the prepolymers and the UV cured hydrogels were characterized by using $^1H$-NMR and FT-IR spectroscopy. Water content, mechanical strength and pore sizes of the hydrogels having different MW of polyols and different ratios of PEG/PTMG were investigated. Hydrogels prepared from PEG(MW1000) only or the mixture of PEG(MW1000) and PTMG(MW2900) with 7:3 by weight were considered as potential candidates for the matrix for the immobilization of microorganism.

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Carbonylative Cyclization of Unsaturated Carboxylic Acids by Palladium Complexes with Phosphines(I) Synthesis and Structure of Palladium(O, II) Complexes with Unsaturated Carboxylic Acids (포스핀류가 배위된 팔라듐 착물에 의한 불포화카르복실산의 카르보닐화고리 반응 (제 1 보). 불포화카르복실산이 배위된 팔라듐(0, Ⅱ) 착물의 합성과 구조)

  • Myung-Ki Doh;Maeng-Jun Jung;Dong-Jin Lee;Kohtaro Osakada;Akio Yamamoto
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.423-430
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    • 1993
  • New Palladium(0)-olefin complexes, $(PMe_3)_2Pd{CH_2=C(CH_3)COOH} \;and\;(PMe_3)_2Pd{(CH_3)CH=CHCOOH}$ have been prepared by treating $Pd(PMe_3)_2$(styrene) with methacrylic acid and trans-crotonic acid, respectively. These complexes were characterized by elemental analysis, IR and $^1H-,\;^{13}C-,\;and\;^{31}P$-NMR spectroscopy. The carboxylic acid entity was found non-bonded with palladium while ${\pi}$-bond is formed between the olefin double bond and Pd(0). The results are compared with the metallacycle formation the reaction of Pd(PMe3)2(styrene) with 3-butenoic acid.

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An NMR Study on the Phase Changes of Lipid Bilayers by Antimicrobial Peptides (항균성 펩타이드에 의한 지질 이중막의 상 변화에 대한 NMR 연구)

  • Kim, Chul
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.183-191
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    • 2010
  • The phase changes of 1-palmitoyl-$d_{31}$-2-oleoyl-sn-glycero-3-phosphatidylcholine (POPC_$d_{31}$) bilayers distorted by an antimicrobial peptide, a magainin 2 or an aurein 3.3 were investigated by using $^2H$ solid-state NMR (SSNMR) spectroscopy. From the theoretical simulation of the experimental $^2H$ solid-state NMR spectra the geometric structure constants and the lateral diffusion coefficients were obtained in the peptide-lipid mixture phases. Within five days of the peptide action on the lipid bilayers only the distorted alignment of the bilayers were measured but after 100 days an elliptic toroidal pore structure and an inverted hexagonal phase were formed in the presence of magainin 2 and aurein 3.3, respectively. In order to investigate the effect of an anionic lipid molecule on the actions of two peptides on the lipid bilayer, the same experiments were performed on the POPC_$d_{31}$/1-palmitoyl-2-oleoyl-sn-glycero-3-phosphatidylglycerol (POPG) bilayer and the significant differences in the actions of two peptides on two bilayers of POPC_$d_{31}$ and POPC_$d_{31}$/POPG were measured.

Biotinoyl Domain of Human Acetyl-CoA Carboxylase;Structural Insights into the Carboxyl Transfer Mechanism

  • Lee, Chung-Kyung;Cheong, Hae-Kap;Ryu, Kyoung-Seok;Lee, Jae-Il;Jeon, Young-Ho;Cheong, Chae-Joon
    • Journal of the Korean Magnetic Resonance Society
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    • v.12 no.1
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    • pp.1-13
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    • 2008
  • Acetyl-CoA carboxylase (ACC) catalyzes the first step in fatty acid biosynthesis: the synthesis of malonyl-CoA from acetyl-CoA. As essential regulators of fatty acid biosynthesis and metabolism, ACCs are regarded as therapeutic targets for the treatment of metabolic diseases such as obesity, In ACC, the biotinoyl domain performs a critical function by transferring an activated carboxyl group from the biotin carboxylase domain to the carboxyl transferase domain, followed by carboxyl transfer to malonyl-CoA. Despite the intensive research on this enzyme, only the bacterial and yeast ACC structures are currently available, To explore the mechanism of ACC holoenzyme function, we determined the structure of the biotinoyl domain of human ACC2 and analyze its characteristics using NMR spectroscopy. The 3D structure of the hACC2 biotinoyl domain has a similar folding topology to the previously determined domains from E. coli and P. Shermanii, however, the 'thumb' structure is absent in the hACC2 biotinoyl domain. Observations of the NMR signals upon the biotinylation indicate that the biotin group of hACC2 does not affect the structure of the biotinoyl domain, while the biotin group for E. coli ACC interacts directly with the thumb residues that are not present in the hACC2 structure. These results imply that, in the E. coli ACC reaction, the biotin moiety carrying the carboxyl group from BC to CT can pause at the thumb of the BCCP domain. The human biotinoyl domain, however, lacks the thumb structure and does not have additional non-covalent interactions with the biotin moiety; thus, the flexible motion of the biotinylated lysine residue must underlie the "swinging arm" motion. This study provides insight into the mechanism of ACC holoenzyme function and supports the "swinging arm" model in human ACCs.

Localization of the Membrane Interaction Sites of Pal-like Protein, HI0381 of Haemophilus influenzae

  • Kang, Su-Jin;Park, Sung Jean;Lee, Bong-Jin
    • Molecules and Cells
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    • v.26 no.2
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    • pp.206-211
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    • 2008
  • HI0381 of Haemophilus influenzae was investigated by circular dichroism (CD) and nuclear magnetic resonance (NMR) spectroscopy. HI0381 is a 153-residue peptidoglycan-associated outer membrane lipoprotein, and a part of the larger Tol/Pal network. Here, we report its backbone $^1H$, $^{15}N$, and $^{13}C$ resonance assignments, and secondary structure predictions. About 97% of all of the $^1HN$, $^{15}N$, $^{13}CO$, $^{13}C{\alpha}$, and $^{13}C{\beta}$ resonances covering 131 non-proline residues of the 134 residue, mature protein, were clarified by sequential and specific assignments. CSI and TALOS analyses revealed that HI0381 contains five ${\alpha}$-helices and five ${\beta}$-strands. To characterize the structure of HI0381, the effects of pH and salt concentration were investigated by CD. In addition, the structural changes occurring when HI0381 was in a membranous environment were investigated by comparing its HSQC spectra and CD data in buffer and in DPC micelles; the results showed that helix ${\alpha}4$ and strand ${\beta}4$ became aligned with the membrane. We conclude that the conformation of HI0381 is affected by the membrane environment, implying that its folded state is directly related to its function.

The Study for Synthesis and Characteristic of ${\alpha},{\beta}$-tetra(phenoxy, 2-naphthoxy, 4-tritylphenoxy) Oxovanadium Phthalocyanine Derivatives (${\alpha},{\beta}$-tetra(phenoxy, 2-naphthoxy, 4-tritylphenoxy) Oxovanadium 프탈로시아닌 유도체의 합성 및 특성에 관한 연구)

  • Son, Dae-Hee;Heo, Jin;Kim, Song-Hyuk;Lee, Seung-Ho;Lee, Gun-Dae;Hong, Seong-Soo;Park, Seong-Soo
    • Applied Chemistry for Engineering
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    • v.21 no.6
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    • pp.638-642
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    • 2010
  • After phthalonitrile derivatives were synthesized by the introduction of phenoxy, 2-naphthoxy or 4-trityl phenoxy group on ${\alpha}$- and ${\beta}$-position, oxovanadyl phthalocyanine (VOPc) derivatives containing electron-rich substituent group at different position were synthesized successfully in this investigation. The chemical structure of samples was determined by the means of $^1H$-NMR, MALDI-TOF mass spectroscopy, and FT-IR spectrometer. Also, optical and chemical properties were determined by the means of UV-Vis spectrometer, X-ray diffractometry, and thermo gravimetry. It was found that the maximum absorbing wavelength of VOPc derivatives ranged from 684 to 726 nm. Also, their solubility and Q-band were enhanced and shifted by the introduction of substitute group, respectively.

Preparation and Characterization of PEG-impregnated Aloe Gel through DIS Processing of Aloe vera Leaf Slice (DIS 공정에 의한 Polyethylene Glycol 함침 알로에 베라 겔의 제조 및 특성화)

  • Kwon, Hye Mi;Hur, Won;Lee, Shin Young
    • KSBB Journal
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    • v.28 no.6
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    • pp.356-365
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    • 2013
  • The novel Aloe gels were prepared with dewatering and impregnation by soaking (DIS) processing of Aloe vera leaf slice at four different temperatures (25, 35, 45 and $55^{\circ}C$), using dehydration solution of 40% (w/v) polyethylene glycol (PEG4000). The PEG-impregnation to Aloe vera leaf slice during DIS was observed depending on immersion temperature, and the PEG-impregnated Aloe vera gel (PEG-i-AVG) obtained was characterized using $^1H$ NMR, FT-IR, GPC, XRD and TGA. The PEG-i-AVG had the higher levels of Aloe bioactives (glucomannan and O-acetyl contents) and better quality indices by $^1H$ NMR and FT-IR spectroscopy than those of native Aloe gel. Also, the obtained Aloe gel maintained the bimodal patterns in higher molecular weight region by GPC indicating no degradation of polysaccharide from native Aloe gel. The result observed by SEM confirmed a surface modification by forming the porous structure, and TGA result exhibited better thermal stability than that of native Aloe gel. XRD result revealed that the crystalline structure in Aloe gel was led by incorporation of PEG. Significant decrease of %insolubility and high enhancement of water solubility index were observed, respectively, and highly ordered conformation such as a helix structure was also indicated by Congo red reaction. We concluded that the modification effect for enhancing function of native Aloe gel was successfully obtained by DIS process using PEG as a dehydrating agent. These results suggested that this DIS process had a high potential for developing a new minimally processed product from Aloe vera leaf.

A Study on the Elucidation of Antimicrobial Activity of Separated Fig Component and the Preparation of Fig Soap (무화과(Fig) 분리 성분의 항균성 규명 및 무화과 비누 제조에 관한 연구)

  • Ryu, Soung-Ryual
    • Journal of the Korean Applied Science and Technology
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    • v.32 no.4
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    • pp.669-684
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    • 2015
  • This study was performed to examine the possibility of Fig extracts for the natural product research. The Fig extracts method were wash, dry and extracted and prepared into two parts; fruit, leaf. The extracts were prepared using alcohol and their chemical structures were estimated by column chromatography, GC-mass spectroscopy, IR, $^1H$-nmr data-base. In order to apply the extracts to hair-care cosmetics, antimicrobial and antifungal ability of the extracts were accomplished using broth serial dilution method. and In order to customer's interest satisfy and test to Fig's industrial propriety of accompany with table luxuries change, The author suggested that to test Fig's industrial property for hand made of transparent and solid soap contained of Fig extracted materials