• 제목/요약/키워드: H-NMR spectroscopy

검색결과 628건 처리시간 0.028초

플라스틱 안경렌즈용 초고굴절 모노머 합성 및 이를 이용한 안경렌즈 제조 (Synthesis of Ultra High Refractive Index Monomer for Plastic Optical Lens and Its Ophthalmic Lens Preparation)

  • 장동규;김종효;이수민;노수균
    • 한국안광학회지
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    • 제13권3호
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    • pp.1-6
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    • 2008
  • 목적: 플라스틱 안경렌즈용 모노머 소재는 거의 전량이 선진국으로부터 국내안경관련 업체가 수입해오고 있는 실정이며 FTA 대비 및 침체되어 가고 있는 안경관련 산업의 활성화를 위해서는 플라스틱 안경렌즈 관련 재료 개발이 절실히 요구되고 있다. 안경렌즈용 소재의 수입대체 효과를 얻기 위해서는 새로운 플라스틱 안경렌즈의 모노머 소재 개발이 절실히 필요하다. 본 연구는 새로운 우레탄계 초고굴절률 플라스틱 안경렌즈 모노머 수지를 합성하고 이를 이용한 안경렌즈 제조한 후, 안경렌즈의 특성을 연구하고자 한다. 방법: 초고굴절용으로 사용가능한 안경렌즈 수지인 ETS-4(2-(2-mercaptoethylthio)-3-{2-[3-mercapto-2-(2-mercaptoethylthio) propylthio]ethylthio}propane-1-thiol)를 합성하고, 이 물질의 확인 및 특성을 연구하기 위해 원소분석, EI-MS, TGA, FT-IR 분광기, ^1H$$^{13}C$ NMR 분광기 등을 이용하였고 모노머 수지와 디이소시아네이트를 혼합하여 균일하게 섞은 후, 안경몰드에 케스팅하고 가열경화하여 얻은 안경렌즈의 광학적인 특성을 조사하기 위해 굴절률 및 아베수를 측정하여 비교하였다. 결과: 합성하고자 하는 소재는 원소분석, EI-MS, TGA, FT-IR 분광기, ^1H$$^{13}C$ NMR 분광기 등의 측정에서 얻은 결과에 의하면 합성되었다는 확인하였고, 합성물질은 세 가지의 이성질체의 존재를 $^{13}C$ NMR 분광법으로 확인 할 수 있다. 아베굴절계로 측정한 액상 상태의 모노머 굴절률은 1.647이었다. ETS-4 모노머 및 디이소시아네이트 종을 이용하여 제조한 안경렌지의 생지는 무색투명하며, 생지의 굴절률은 1.656~1.680 이었다. 결론: 새로운 초고굴절용 플라스틱 안경렌즈의 모노머를 합성하고, 그 물질의 구조 및 특성을 연구하였다. 이를 이용하여 제조한 플라스틱 안경렌즈는 무색투명하며 특성이 우수하여 상업화가 가능하다.

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Synthesis and Characterization of New Group 13 Complexes of 2-Acetylpyridine-S-methyldithiocarbazate. Single-Crystal Structure of Me₂Ga[$NC_5H_4C$(CH₃)NNC(S)SMe] and Me₂In[$NC_5H_5C$(CH₃)NNC(S)SMe]

  • 백철기;강상욱;이채호;이영행;고재정
    • Bulletin of the Korean Chemical Society
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    • 제18권3호
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    • pp.311-316
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    • 1997
  • The synthesis and characterization of the mononuclear group 13 heterocyclic carboxaldehyde methyldithiocarbazate complexes Me2M[NC5H4CRNNC(S)SCH3] (M=Al, R=H(1); M=Ga, R=H(2); M=Al, R=CH3(3); M-Ga, R=CH3(4); M=In, R=CH3(5)) are described. Compounds 1-5 were prepared by the reaction of MMe3 (M=Al, Ga, In) with 2-formy or 2-acetylpyridine-S-methyldithiocarbazate in toluene. These compounds 1-5 have been characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and single-crystal X-ray diffraction. X-ray single-crystal diffraction analyses reveal that 4-5 are mononuclear metal compounds with coordination number of 5 and N,N,S coordination mode.

Purification and Structural Characterization of Cold Shock Protein from Listeria monocytogenes

  • Lee, Ju-Ho;Jeong, Ki-Woong;Kim, Yang-Mee
    • Bulletin of the Korean Chemical Society
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    • 제33권8호
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    • pp.2508-2512
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    • 2012
  • Cold shock proteins (CSPs) are a family of proteins induced at low temperatures. CSPs bind to single-stranded nucleic acids through the ribonucleoprotein 1 and 2 (RNP 1 and 2) binding motifs. CSPs play an essential role in cold adaptation by regulating transcription and translation via molecular chaperones. The solution nuclear magnetic resonance (NMR) or X-ray crystal structures of several CSPs from various microorganisms have been determined, but structural characteristics of psychrophilic CSPs have not been studied. Therefore, we optimized the purification process to obtain highly pure Lm-Csp and determined the three-dimensional structure model of Lm-Csp by comparative homology modeling using MODELLER on the basis of the solution NMR structure of Bs-CspB. Lm-Csp consists of a ${\beta}$-barrel structure, which includes antiparallel ${\beta}$ strands (G4-N10, F15-I18, V26-H29, A46-D50, and P58-Q64). The template protein, Bs-CspB, shares a similar ${\beta}$ sheet structure and an identical chain fold to Lm-Csp. However, the sheets in Lm-Csp were much shorter than those of Bs-CspB. The Lm-Csp side chains, E2 and R20 form a salt bridge, thus, stabilizing the Lm-Csp structure. To evaluate the contribution of this ionic interaction as well as that of the hydrophobic patch on protein stability, we investigated the secondary structures of wild type and mutant protein (W8, F15, and R20) of Lm-Csp using circular dichroism (CD) spectroscopy. The results showed that solvent-exposed aromatic side chains as well as residues participating in ionic interactions are very important for structural stability. Further studies on the three-dimensional structure and dynamics of Lm-Csp using NMR spectroscopy are required.

NMR Spectroscopic Analysis on the Chiral Recognition of Noradrenaline by β-Cyclodextrin ( β-CD) and Carboxymethyl- β-cyclodextrin (CM- β-CD)

  • Lee, Sang-Hoo;Yi, Dong-Heui;Jung, Seung-Ho
    • Bulletin of the Korean Chemical Society
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    • 제25권2호
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    • pp.216-220
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    • 2004
  • ${\beta}$-CD and CM- ${\beta}$-CD as chiral NMR shift agents were used to resolve the enantiomers of noradrenaline (NA). The stoichiometry of each complex formed between the CDs and the enantiomers of NA was found to be 1 : 1 through the continuous variation plots. The binding constants (K) of the complexes were determined from $^1H$ NMR titration curves. This result indicated that both ${\beta}$-CD and CM- ${\beta}$-CD formed the complexes with the S(+)-NA more preferentially than its R(-)-enantiomer. The K values for the complexes with ${\beta}$-CD ($K_{S(+)}$ = 537 $M^{-1}$ and $K_{R(-)}$ = 516 $M^{-1}$ was larger than those with CM- ${\beta}$-CD ($K_{S(+)}$ = 435 $M^{-1}$ and $K_{R(-)}$ = 313 $M^{-1}$), however, enantioselectivity (${\alpha}$) of S(+)- and R(-)-NA to CM- ${\beta}$-CD ( ${\alpha}$ = 1.38) was larger than that to ${\beta}$-CD ( ${\alpha}$ = 1.04), indicating that CM- ${\beta}$-CD was the better chiral NMR solvating agents for the recognition of the enantiomers of NA. Two dimensional rotating frame nuclear Overhauser enhancement spectroscopy (ROESY) experiments were also performed to explain the binding properties in terms of spatial fitting of the NA molecule into the macrocyclic cavities.

가시오갈피 유식물체 추출물의 항산화 활성물질 (Antioxidative Compounds in Extracts of Eleutherococcus senticosus Max. Plantlets)

  • 김명조;권용수;유창연
    • 한국약용작물학회지
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    • 제13권4호
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    • pp.194-198
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    • 2005
  • 가시오갈피 유식물체의 함유성분을 밝히고, 분리된 화합물들을 대상으로 DPPH를 이용한 항산화활성을 측정하여 대체 약용자원으로서의 사용 가능성을 검토하기 위하여 가시오갈피 유식물체를 MeOH로 추출, 농축하고 Hexane, EtOAc 및 BuOH순으로 분획하여 얻은 각각의 분획을 대상으로 성분연구에 착수하였다. 각종 column chromatography를 이용하여 성분을 분리한 결과 EtOAc분획으로부터 1종의 화합물을 분리하였고, BuOH 분획으로부터 1종의 화합물을 분리하였다. 이들 화합물에 대하여 UV, IR, Mass, $^1H-NMR$$^{13}C-NMR$ spectrum과 문헌치를 대조하여 그 구조를 동정한 결과그 구조는 각각 Chlorogenic acld (1)과 1,4-di-O-caffeoyl-quinic acid (2)이였다. DPPH (1,1-diphenyl-2-picry-hydrazyl) free radical scavenging activity를 이용하여 측정한 항산화활성의 $RC_{50}$ value는 각각 1.2 및 $0.4\;{\mu}g/ml$였다. 이상의 결과로부터 가시오갈피 유식물체 (Eleutherococcus senticosus Max.)는 천연 항산화제로서의 개발가능성이 높다고 사료된다.

Color Alteration and Acaricidal Activity of Juglone Isolated from Caesalpinia sappan Heartwoods Against Dermatophagoides spp.

  • Lee, Chi-Hoon;Lee, Hoi-Seon
    • Journal of Microbiology and Biotechnology
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    • 제16권10호
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    • pp.1591-1596
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    • 2006
  • Acaricidal effects of materials derived from Caesalpinia sappan heartwoods against Dermatophagoides farinae and D. pteronyssinus were assessed and compared with those evidenced by commercial benzyl benzoate and DEET. The observed responses varied according to dosage and mite species. The $LD_{50}$ values of the methanol extracts derived from C. sappan heartwoods were 6.13 and $5.44{\mu}g/cm^3$ against D. farinae and D. pteronyssinus, respectively. Furthermore, the ethyl acetate fraction derived from the methanol extract was approximately 8.71 more toxic than DEET against D. farinae, and 4.73 times more toxic against D. pteronyssinus. The biologically active constituent from the ethyl acetate fraction of C. sappan heartwood extract was purified via silica gel chromatography and high-performance liquid chromatography. The structure of the acaricidal component was analyzed by $GC-MS,\;^1H-NMR,\;^{13}C-NMR,\;^1H-^{13}C\;COSY-NMR$, and DEPT-NMR spectroscopy, and identified as juglone (5-hydroxy-l,4-naphthoquinone). Based on the $LD_{50}$ values of juglone and its derivatives, the most toxic compound against D. farinae was juglone ($0.076{\mu}g/cm^3$), followed by benzyl benzoate ($9.143{\mu}g/cm^3$) and 2methyl-l,4-naphthoquinone ($40.0{\mu}g/cm^3$). These results indicate that the acaricidal activity of C. sappan heartwoods is likely to be the result of the effects of juglone. Additionally, juglone treatment was shown to effect a change in the color of the cuticles of house dust mites, from colorless-transparent to dark brownish-black. Accordingly, as a naturally occurring acaricidal agent, C. sappan heartwood-derived juglone should prove to be quite 'useful as a potential control agent, lead compound, and house dust mite indicator.

NMR Studies on the Structure of Human Annexin I

  • Han, Hee-Yong;Bang, Keun-Su;Na, Doe-Sun;Lee, Bong-Jin
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 1996년도 춘계학술대회
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    • pp.182-182
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    • 1996
  • Annexin I is a member of the annexin family of calcium dependent phospholipid binding proteins and has anti-inflammatory activity by inhibiting phospholipase A$_2$ (PLA$_2$). Recent X-ray crystallographic study of annexin I identified six Ca$\^$2+/ binding bites, which was different types (type II, III) from the well-known EF-hand motif (type I). In this work, the structure of annexin I was studied at atomic level by using $^1$H, $\^$15/N and $\^$l3/C NMR(nuclear magnetic resonance) spectroscopy, and the effect of Ca$\^$2+/ binding on the structure of annexin I was studied, and compared with that of Mg$\^$2+/ binding, When Ca$\^$2+/ was added to annexin I, NMR peak change was occured in high- and low-field regions of $^1$H-NMR spectra. NMR peak change by Ca$\^$2+/ binding was different from that by Mg$\^$2+/ binding. Because annexin I is a larger protein with 35 kDa molecular weight, site-specific (amide-$\^$15/N, carbonyl-$\^$l3/C) labeling technique was also used. We were able to detect methionine, tyrosine and phenylalanine peaks respectively in $\^$13/C-NMR spectra, and each residue was able to be assigned by the method of doubly labeling annexin I with [$\^$13/C] carbonyl-amino acid and [$\^$15/N] amide-amino acid. In $\^$l3/C-NMR spectra of [$\^$13/C] carbonyl-Met labeled annexin I, we observed that methionine residues spatially located near Ca$\^$2+/ binding Sites Were Significantly effected by Ca$\^$2+/ binding. From UV spectroscopic data on the effect of Ca$\^$2+/ binding, we knew that Ca$\^$2+/ binding sites of annexin I have cooperativity in Ca$\^$2+/ binding. The interaction of annexin I with PLA$_2$ also could be detected by using heteronuclear NMR spctroscopy. Consequently, we expect that the anti-inflammatory action mechanism of annexin I may be a specific protein-protein interaction. The residues involved in the interaction with PLA$_2$ can be identified as active site by assigning NMR peaks effected by PLA$_2$ binding.

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Syntheses and Theoretical Study of Palladium(II) Complexes with Aminophosphines as 7-Membered Chelate Rings

  • 김봉곤;양기열;정맹준;이배욱;도명기
    • Bulletin of the Korean Chemical Society
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    • 제18권11호
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    • pp.1162-1166
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    • 1997
  • Nature of palladium(Ⅱ) complexes with 7-membered chelates was studied by experimental and theoretical methods on a Pd(L)Cl2 system, where L is Ph2PNHCH2CH2NHPPh2(L1), Ph2PNHC6H4NHPPh2(L2). The palladium(Ⅱ) complexes were prepared and characterized by elemental analysis, IR, UV, 1H, and 31P NMR spectroscopy. Ab initio calculations with geometry optimizations were also performed for related model systems, Pd(L)Cl2; L=R2PNH(CH2)2NHPR2(L3), R2PNHC6H4NHPR2(L4), R2P(CH2)4PR2(L5), R2PCH2(C6H4)CH2PR2(L6); R=H, CH3.

Nitrogen-doped carbon nanosheets from polyurethane foams and removal of Cr(VI)

  • Duan, Jiaqi;Zhang, Baohua;Fan, Huailin;Shen, Wenzhong;Qu, Shijie
    • Carbon letters
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    • 제22권
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    • pp.60-69
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    • 2017
  • Nitrogen-doped carbon nanosheets with a developed porous structure were prepared from polyurethane foams by hydrothermal carbonization following $ZnCl_2$ chemical activation. Scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, solid state $^{13}C$ nuclear magnetic resonance (NMR) spectra and X-ray photoelectron spectroscopy were used to characterize the nitrogen-doped carbon nanosheet structure and composition. The removal of Cr(VI) by the N-doped carbon nanosheets was investigated. The results showed that the maximum removal capacity for chromium of 188 mg/g was found at pH=2.0 with PHC-Z-3. pH had an important effect on Cr(VI) removal and the optimal pH was 2.0. Moreover, amino groups and carboxyl groups in the nitrogen-doped carbon nanosheet played important roles in Cr(VI) removal, and promoted the reduction of Cr(VI) to Cr(III).

Synthesis and Characterization of Low Molecular Weight Poly(methyl acrylate)-b-Polystyrene by a Combination of ATRP and Click Coupling Method

  • Hasneen, Aleya;Kim, Su-Jeong;Paik, Hyun-Jong
    • Macromolecular Research
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    • 제15권6호
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    • pp.541-546
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    • 2007
  • The combination of atom transfer radical polymerization (ATRP) and click chemistry was employed for the efficient preparation of well-defined block copolymers. Bromo terminated poly(methyl acrylate) (pMA-Br) was prepared by an ATRP initiator, ethyl-2-bromoisobutyrate (EBiB). Subsequently, the bromine chain end of pMA-Br was converted to an azide group by simple nucleophilic substitution reaction. ${\alpha}-Alkyn-{\omega}-bromo-functionalized$ polystyrene was also synthesized by ATRP using the alkyn-functionalized initiator, propargyl-2-bromoisobutyrate (PgBiB). In both cases, the conversion was limited to a low level to ensure a high degree of chain end functionality. Then the coupling reaction between the azide end group in $pMA-N_3$ and alkyn-functionalized PgBiB-pSt was performed by Cu(I)catalysis. This coupling reaction was monitored by gel permeation chromatography (GPC). The synthesized block copolymer was characterized by FT-IR, $^1H-NMR$ spectroscopy and $^1H-^1H$ COSY correlation spectroscopy.