• 제목/요약/키워드: $^1H$-nmr spectrum

검색결과 231건 처리시간 0.029초

인쇄문화사에 대한 고찰 - 진주지역을 중심으로 (Study on the History of Printing Culture - The Center of Jin-Ju Areas -)

  • 장추남
    • 한국인쇄학회지
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    • 제13권2호
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    • pp.47-53
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    • 1995
  • Photosensitive resin of azide type is good for resolution and inner solvent, but it is really problem to development of practical use because fanctional groups of polymer has many hydrophilic radicals. By careful attention to this point, this study was investigated synthesis term, photo property and development property of composed photosensitive resin of azida type, it is to this effect. 1) H-NMR spectrum of compared DABCI showed amion redical by $\delta$6.0~6.1ppm to substitude for azide radical by amino radical by $\delta$8.9~9.45ppm, and FT-IR absorption spectra showed the absorption bends at 2100cm. 2)FT-IR absorption spectra of PHS1-DAB, PHS2-DAB, CMM-DAB and CHM-DAB showed azida radical pick to be lost at after irradiation by UV light. 3) According to exposuer change of PHS1-DAB, PHS2-DAB, CMM-DAB and CHM-DAB, absorption maximum value of UV spectrum change was 280nm. 4) to compared relative sensitivity of compared photosensitive resin, PHS2-DAB was the best and to compared insolubility rate of compared photosensitive resin, CMM-DAB was the lower. 5)Solubility if NaOH was the best by 1.0mol/$\ell$ and solubility of developing solution of ethanol to water was it in the ratio of 4 to 1.

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A New Model for the Reduced Form of Purple Acid Phosphatase: Structure and Properties of $[Fe_2BPLMP(OAc)_2](BPh_4)_2$

  • 임선화;이진호;이강봉;강성주;허남휘;Jang, Ho G.
    • Bulletin of the Korean Chemical Society
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    • 제19권6호
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    • pp.654-660
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    • 1998
  • $[Fe^{II}Fe^{III}BPLMP(OAc)_2](BPh_4)_2$ (1), a new model for the reduced form of the purple acid phosphatases, has been synthesized by using a dinucleating ligand, 2,6-bis[((2-pyridylmethyl)(6-methyl-2-pyridylmethyl)amino) methyl]-4-methylphenol (HBPLMP). Complex I has been characterized by X-ray diffraction method as having (μ-phenoxo)bis(acetato)diiron core. Complex 1 was crystallized in the monoclinic space group C2/c with the following cell parameters: a=41.620(6) Å, b=14.020(3) Å, c=27.007(4) Å, β=90.60(2)°, and Z=8. The iron centers in the complex 1 are ordered as indicated by the difference in the Fe-O bond lengths which match well with typical $Fe^{III}-O\; and\; Fe^{II}-O$ bond lengths. Complex 1 has been studied by electronic spectral, NMR, EPR, SQUID, and electochemical methods. Complex 1 exhibits strong bands at 592 nm, 1380 nm in $CH_3CN$ (ε = 1.0 × 103 , 3.0 × 102). These are assigned to $phenolate-to-Fe^{III}$ and intervalence charge-transfer transitions, respectively. Its NMR spectrum exhibits sharp isotropically shifted resonances, which number half of those expected for a valence-trapped species, indicating that electron transfer between $Fe^{II}\;and\;Fe^{III}$ centers is faster than NMR time scale. This complex undergoes quasireversible one-electron redox processes. The $Fe^{III}_2/Fe^{II}Fe^{III}\;and\;Fe^{II}Fe^{III}/Fe^{II}_2$ redox couples are at 0.655 and -0.085 V vs SCE, respectively. It has $K_{comp}=3.3{\times}10^{12}$ representing that BPLMP/bis(acetate) ligand combination stabilizes a mixed-valence $Fe^{II}Fe^{III}$ complex in the air. Complex 1 exhibits a broad EPR signal centered near g=1.55 which is a characteristic feature of the antiferromagnetically coupled high-spin $Fe^{II}Fe^{III}$ system $(S_{total}=1/2)$. This is consistent with the magnetic susceptibility study showing the weak antiferromagnetic coupling $(J= - 4.6\;cm^{-1},\; H= - 2JS_1{\cdot}S2)$ between $Fe^{II}\; and \;Fe^{III}$center.

열처리 양파로부터 항산화물질의 분리동정 (Isolation and Identification of an Antioxidant Substance from Heated Onion (Allium cepa L.))

  • 황인국;김현영;이상훈;황초롱;오승희;우관식;김대중;이준수;정헌상
    • 한국식품영양과학회지
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    • 제40권3호
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    • pp.470-474
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    • 2011
  • 열처리한 양파 착즙액의 ethyl acetate 분획물로부터 항산화물질을 분리 동정하기 위하여 1, 2차 silica gel column chromatography, preparative TLC 및 HPLC를 이용하여 항산화활성 물질을 분리 정제하였다. GC/MSD, $^1H$-NMR 및 $^{13}C$-NMR spectrum 결과로부터 구조 동정한 결과 분리된 물질은 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one(DDMP)으로 확인되었다. DDMP의 항산화활성의 $IC_{50}$값은 241.6 ${\mu}g/mL$이었으며, vitamin E의 69.2 ${\mu}g/mL$와 C의 45.3 ${\mu}g/mL$보다는 낮은 활성을 보였고 BHT의 268.0 ${\mu}g/mL$보다는 높은 활성을 보였지만 유의적인(p>0.05) 차이는 나타나지 않았다. 추후 DDMP를 기능성물질로 활용하기 위하여 다양한 생리활성 평가가 필요할 것으로 생각된다.

Solution Structure of Water-soluble Mutant of Crambin and Implication for Protein Solubility

  • Kang, Su-Jin;Lim, Jong-Soo;Lee, Bong-Jin;Ahn, Hee-Chul
    • Bulletin of the Korean Chemical Society
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    • 제32권5호
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    • pp.1640-1644
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    • 2011
  • Water-soluble mutant of intrinsically insoluble protein, crambin, was produced by mutagenesis based on the sequence analysis with homologous proteins. Thr1, Phe13, and Lys33 of crambin were substituted for Lys, Tyr, and Lys, respectively. The resultant mutant was soluble in aqueous buffer as well as in dodecylphosphocholine (DPC) micelle solution. The $^1H-^{15}N$ spectrum of the mutant crambin showed spectral similarity to that of the wild-type protein except for local regions proximal to the sites of mutation. Solution structure of water-soluble mutant crambin was determined in aqueous buffer by NMR spectroscopy. The structure was almost identical to the wild-type structure determined in non-aqueous solvent. Subtle difference in structure was very local and related to the change of the intra- and inter-protein hydrophobic interaction of crambin. The structural details for the enhanced solubility of crambin in aqueous solvent by the mutation were provided and discussed.

Molecular Cloning and NMR Characterization of the Nonreceptor Tyrosine Kinase PTK6 SH3-SH2-Linker Domain

  • Lee, Young-Min;Ahn, Kyo-Eun;Ko, Sung-Geon;Lee, Weon-Tae
    • Bulletin of the Korean Chemical Society
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    • 제30권5호
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    • pp.1043-1046
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    • 2009
  • Human protein tyrosine kinase-6 (PTK6) is a member of the non-receptor protein tyrosine kinase family and it is found in two-thirds of all breast tumors. Very recently, we proposed that the SH3 domain of PTK6 interacts with the linker region (Linker) between the SH2 and kinase domains, proving that the interaction between SH3 domain and Linker plays an important role in auto-inhibition mechanism. Residues from 1 to 191 corresponding region of SH3-SH2-Linker (SH32L) of PTK6 was cloned into the pET32a expression vector with Tobbaco etch virus (TEV) protease enzyme site by sequence homology and 3D structural model. The purified PTK6-SH32L was determined as a monomer conformation in solution. The amide proton resonances in the $^{15}N-^{1}H$ 2D-HSQC spectrum suggest that PTK6-SH32L possesses disordered structural region of the flexible/unstructured linker region. In addition, the backbone amide proton chemical shifts of the SH3 domain in the PTK6-SH32L differ from that of the independent domain, indicating that intra-molecular interaction between SH3 and Linker in the PTK6-SH32L is present.

동부로부터 sterol의 분리 동정 (Sterols from the Seed of Cowpea (Vigna sinensis K.))

  • 최은희;박희정;오청;정인식;김지영;백남인
    • Journal of Applied Biological Chemistry
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    • 제53권2호
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    • pp.77-81
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    • 2010
  • 동부를 80% MeOH로 추출하고, 얻어진 추출물을 EtOAc, n-BuOH 및 $H_2O$로 용매 분획 하였다. 이 중 EtOAc과 n-BuOH 분획으로부터 silica gel과 octadecyl silica gel(ODS) column chromatography를 반복하여 4종의 sterol 화합물을 분리, 정제하였다. 각 화합물의 화학구조는 NMR, MS 및 IR 등의 spectrum data를 해석하여, stigmasterol(1a), $\beta$-sitosterol(1b), 7-ketositosterol(2) 및 stigmasterol 3-O-$\beta$-D-glucopyranoside(3)로 동정하였다. 화합물 1b, 2와 3은 동부에서 처음 분리되었다.

제주도 재래감귤의 식물학적 특성과 이용에 관한 연구 (II) -병귤(甁橘)의 성분연구- (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-)

  • 김창민;허인옥;한대석
    • 생약학회지
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    • 제10권2호
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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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A New Functional Model Complex of Extradiol-cleaving Catechol Dioxygenases: Properties and Reactivity of [$Fe^{II}$(BLPA)DBCH]BPh₄

  • Lim, Ji H.;Park, Tae H.;이호진;이강봉;Jang, Ho G.
    • Bulletin of the Korean Chemical Society
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    • 제20권12호
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    • pp.1428-1432
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    • 1999
  • [Fe$^{II}$(BLPA)DBCH]BPh₄ (1), a new functional model for the extradiol-cleaving catechol dioxygenases, has been synthesized, where BLPA is bis(6-methyl-2-pyridylmethyl)(2-pyridylmethyl)amine and DBCH is 3,5-di-tert-butylcatecholate monoanion. ¹H NMR and EPR studies confirm that 1 has a high-spin Fe(II) (S = 2) center. The electronic spectrum of 1 exhibits one absorption band at 386 nm, showing the yellow color of the typical [Fe$^{II}$(BLPA)] complex. Upon exposure to O₂, 1 is converted to an intense blue species within a minute. This blue species exhibits two intense bands at 586 and 960 nm and EPR signals at g = 5.5 and 8.0 corresponding to the high-spin Fe(III) complex (S = 5/2, E/D = 0.11). This blue complex further reacts with O₂ to be converted to (μ-oxo)Fe$^{III}_2$ complex within a few hours. Interestingly, 1 affords intradiol cleavage (65%) and extradiol cleavage (20%) products after the oxygenation. It can be suggested that 1 undergoes two different oxygenation pathways. The one takes the substrate activation mechanism proposed for the intradiol cleavage products after the oxidation of the $Fe^II\;to\;Fe^{III}$. The other involves the direct attack of O₂ to $Fe^{II}$ center, forming the $Fe^{III}$-superoxo intermediate which can give rise to the extradiol cleavage products. 1 is the first functional Fe(II) complex for extradiol-cleaving dioxygenases giving extradiol cleavage products.

Phellodendron amurense의 미백물질을 이용한 화장품 특성 (Characteristics of Cosmetic with Whitening Compounds from Phellodendron amurense)

  • 조영제
    • Journal of Applied Biological Chemistry
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    • 제54권2호
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    • pp.108-113
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    • 2011
  • 황백 추출물의 tyrosinase 억제효과를 검토한 결과 60% 에탄올추출물에서 25% 정도의 억제효과를 나타내었으며, melanoma세포(B16F10)에서의 멜라닌 생합성을 측정한 결과 31.2%의 저해활성을 나타내어 멜라닌생성억제효과가 있음을 알 수 있었다. 황백추출물에서 tyrosinase저해 활성물질을 정제하고자 Sephadex LH-20과 MCI-gel CHP-20 open column을 이용하여 용출한 결과 순수하게 정제된 활성물질을 얻을 수 있었으며, 정제물질을 구조 동정한 결과 미백물질은 obacunone으로 동정되었다. 정제된 obacunone은 35.1%의 저해활성을 나타내어 미백 활성이 비교적 우수함을 확인할 수 있었으며, 황백추출물로부터 분리한 미백물질을 이용한 미백 화장품을 제조하여 관능평가를 한 결과 우수한 평가를 받았다. 미백화장품의 안정성 검사를 위해 pH, 점도 및 복소탄성률의 변화를 측정하였으나 저장기간 60일 동안 큰 변화를 나타내지 않았다. 또한 온도변화, 인공 및 자연광에 의한 변화, 온도순환에 의한 변화 및 냉 해동순환(Freeze & Thaw cycling)에 따른 변화들 살펴본 결과 저장 60일 동안 모든 조건에서 상의 분리와 변색, 변취 등의 변화 없이 안정성을 나타내었다.

Acetoacetanilide 유도체 합성 (Studies on the Synthesis of Acetoacetanilide Derivatives)

  • 김인규
    • 대한화학회지
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    • 제25권1호
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    • pp.44-49
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    • 1981
  • Acetoacetanilide를 브롬화한 결과 예상한 ${\alpha}$-bromo 유도체가 얻어지지 않고, r-bromo 유도체가 얻어졌다. 이것을 mercaptoethanol과 반응시켜 sulfide 유도체를 만든다음, 산성하에서 고리화시킨 결과 2-(N-phenylcarbamoyl)methylene-1,4-oxathiane이 좋은 수율로 얻어졌다. 이 물질은 살균제 농약으로 널리 사용되고 있는 carboxin과 그 구조가 매우 유사하므로 이 물질의 biological activity는 흥미있는 과제가 될 것이다.

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