• 제목/요약/키워드: 1D $^1H-NMR$

검색결과 639건 처리시간 0.03초

재생자원 유래 퓨란계 에폭시 화합물의 합성 및 접착 특성 (Synthesis of Renewable Resource-derived Furan-based Epoxy Compounds and Their Adhesive Property)

  • 이재성;이상협;정재원;김백진;조진구;김현중
    • 접착 및 계면
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    • 제11권2호
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    • pp.41-49
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    • 2010
  • 탄소 중립형 친환경 접착소재로서, 퓨란기를 함유하는 에폭시 단량체(8, 9)를 설계하고 합성하였다. 바이오매스로부터 바이오-리파이너리 공정을 통해 쉽게 얻을 수 있는 퓨란과 메틸 아크릴레이트를 출발물질로 하여 Diels-Alder 반응을 통하여 이중고리 뼈대를 합성하였다. 이후 에스테르 작용기를 알코올로 환원한 후 에피클로로하이드린과 반응하여 에폭시기를 함유하는 새로운 퓨란계 단량체(8, 9)를 합성하였다. 구조는 $^1H$ and $^{13}C$ NMR으로 확인하였으며, UV 경화형 단량체로서의 기본적인 성질인 광경화 속도 및 광경화율은 Photo-DSC를 사용하여 확인하였다. 또한 선형가변 미분변환기(Linear Variable Differential Transformer transducer LVDT)와 UV Spot curing 장비를 통해 화합물의 경화 수축율을 측정하여 화합물의 분자구조가 경화수축율에 미치는 영향을 살펴보았으며, 각 합성 화합물을 폴리카보네이트 피착재 사이에 도포하고 광경화 후 lab shear test를 수행한 결과 3 MPa 이상의 전단강도를 보임으로써 재생자원 유래 신규 화합물이 접착소재로서 적용이 가능하다는 것을 확인하였다.

기능성 순간접착제용 중합체 첨가제의 제조 및 특성 (Preparation and Characteristics of Polymer Additives for Functional Instant Adhesives)

  • 임혜정;안광덕;김성범;김의용;한동근
    • 접착 및 계면
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    • 제2권3호
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    • pp.25-32
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    • 2001
  • 순간접착제로 사용되고 있는 에틸 시아노아크릴레이트(ECA) 단량체는 개시제 없이 공기중의 수분에 의해서 쉽게 중합이 될 수 있어서 산업용 및 가정용 접착제로 응용되고 있다. 그러나 ECA 단량체는 그 자체가 가지는 저점도성으로 인해서 피착제 내부로 흘러들어가는 단점을 가지고 있다. 이를 보완하기 위해서 상업적으로 폴리메틸메타크릴레이트(PMMA)를 첨가하고 있지만 PMMA의 사용은 순간접착제의 유연성을 감소시키는 결과를 초래한다. 또한 순간접착제의 중합체는 취약하다는 문제점을 가지고 있다. 본 연구에서는 기존 순간접착제 단량체의 중점성과 중합체의 유연성을 동시에 부여할 수 있는 새로운 PMMA 함유 중합체의 기능성 첨가제를 제조하였다. 즉, 유리전이온도(Tg)가 낮은 비닐 아세테이트(VAc)와 에틸비닐에테르(EVE)를 MMA와 라디칼 중합을 행하여 P(MMA-VAc)와 P(MMA-VAc-EVE)의 기능성 첨가제를 얻었다. 제조된 첨가제는 ECA 단량체에 첨가시켜 기능성을 갖는 순간접착제를 제조하였다. 첨가제 및 ECA 중합체의 구조는 $^1H$ NMR 및 FTIR로 확인하였으며 각각의 물리적 및 기계적 물성을 평가하였다. 얻어진 첨가제의 Tg는 VAc나 VAc-EVE가 증가할수록 감소하여 유연성을 나타내었고 첨가제가 함유된 기능성 순간접착제는 기존 PMMA만이 함유된 순간접착제에 비해 더 높은 접착강도를 보였다.

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Identification of 5-Hydroxy-3,6,7,8,3',4'-Hexamethoxyflavone from Hizikia fusiforme Involved in the Induction of the Apoptosis Mediators in Human AGS Carcinoma Cells

  • Kim, Min Jeong;Lee, Hye Hyeon;Seo, Min Jeong;Kang, Byoung Won;Park, Jeong Uck;Kim, Kyoung-Sook;Kim, Gi-Young;Joo, Woo Hong;Choi, Yung Hyun;Cho, Young-Su;Jeong, Yong Kee
    • Journal of Microbiology and Biotechnology
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    • 제22권12호
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    • pp.1665-1672
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    • 2012
  • An 80% ethanol extract of Hizikia fusiforme was obtained and followed by successive fractionation using the organic solvents n-hexane, ethyl acetate, and n-butanol to identify the antioxidative substance. The aqueous part of the nbutanol fractionation step, showing high antioxidative activity, was subjected to reverse-phase liquid chromatography. As a result, a substance purified from a BB-2 fraction showed high antioxidative activity. The m/z 419 [M+H] molecular ion peak in the fraction was observed by the analysis of the ESI-LC/MS spectrum. By the analysis of 1H NMR (500 MHz, DMSO-$d_6$) and $^{13}C$ NMR (125 MHz, DMSO-$d_6$) spectra, a unique compound of the fraction was biochemically identified as a 5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone (5HHMF). We also investigated the effect of 5HHMF on human gastric AGS carcinoma cells. Western blot analysis suggested that the flavone substantially increased the levels of the death receptor-associated apoptosis mediators Fas, Fas L, FADD, TRADD, and DR4 in a concentration-dependent manner. The levels of Fas, Fas L, TRADD, and DR4 in the cells treated with 5HHMF ($5{\mu}g/ml$) were approximately 26.4-, 12.8-, 6.7-, and 9.8-times higher than those of non-treated cells, respectively. Of note, the level of FADD protein in the cells exposed to 5HHMF ($1{\mu}g/ml$) increased approximately 9.6-times. In addition, the cleavage of caspase-3, -8, and -9 in cultured AGS cells treated with 5HHMF was significantly confirmed. Therefore, our results suggest that 5HHMF from H. fusiforme is involved in the induction of death receptor-associated apoptosis mediators in human gastric AGS carcinoma cells.

Screening and Identification of Antimicrobial Compounds from Streptomyces bottropensis Suppressing Rice Bacterial Blight

  • Park, Sait-Byul;Lee, In-Ae;Suh, Joo-Won;Kim, Jeong-Gu;Lee, Choong-Hwan
    • Journal of Microbiology and Biotechnology
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    • 제21권12호
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    • pp.1236-1242
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    • 2011
  • Xanthomonas oryzae pv. oryzae (Xoo) is the most devastating pathogen to Oryza sativa and has been shown to cause bacterial blight. Two bioactive compounds showing antimicrobial activities against Xoo strain KACC 10331 were isolated from a Streptomyces bottropensis strain. The ethyl acetate extract was fractionated on a Sephadex LH-20 column, and then purified by preparative HPLC. The purified compounds were identified as bottromycin A2 and dunaimycin D3S by HR/MS and $^1H$ NMR analyses. The MIC value against Xoo and the lowest concentration still capable of suppressing rice bacterial blight were 2 ${\mu}g$/ml and 16 ${\mu}g$/ml for bottromycin A2, and 64 ${\mu}g$/ml and 0.06 ${\mu}g$/ml for dunaimycin D3S, respectively. These two compounds were shown to exert different bioactivities in vitro and in rice leaf explants.

Synthesis, Urease and Acetylcholine Esterase Inhibition Activities of Some 1,4-Disubstituted Thiosemicarbazides and their 2,5-Disubstituted Thiadiazoles

  • Saleem, Muhammad;Rafiq, Muhammad;Hanif, Muhammad;Rama, Nasim Hasan;Seo, Sung-Yum;Lee, Ki-Hwan
    • Bulletin of the Korean Chemical Society
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    • 제33권8호
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    • pp.2741-2747
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    • 2012
  • A new series of 2,5-disubstituted-1,3,4-thiadiazoles 6a-i was synthesized by overnight stirring various 1,4-disubstituted thiosemicarbazides 5a-i in polyphosphoric acid followed by neutralization. The structures of newly synthesized compounds 5a-i and 6a-i were characterized by IR, $^1H$ and $^{13}C$ NMR, elemental analysis and mass spectrometric studies. All the synthesized compounds were evaluated for their urease and acetylcholine esterase inhibition activities. Thiosemicarbazides 5a-i are found to possess excellent potential for urease inhibition, more than the standard drug. Thiosemicarbazides 5a-i are more potent urease inhibitor than their cyclic analogues thiadiazoles 6a-i. Almost all of the compounds are excellent inhibitors of acetylcholine esterase. The inhibition of acetylcholine esterase of compounds 5a, 5c, 5d, 5g, 5i, 6e, 6f, 6g, and 6i is much more than that of standard drug.

식용식물자원으로부터 활성물질의 탐색-XVII. 싸주아리쑥(Artemisia princeps PAMPANINI, Sajuarissuk) 지상부의 화학성분 (Development of Biologically Active Compounds from Edible Plant Sources-XVII. Chemical Constituents from the Aerial Parts of Artemisia princeps PAMPANINI (Sajuarissuk))

  • 유종수;방면호;안은미;송명종;정해곤;정태숙;이경태;최명숙;백남인
    • Applied Biological Chemistry
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    • 제50권1호
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    • pp.53-56
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    • 2007
  • 싸주아리쑥 지상부를 80% MeOH 용액으로 추출하고, 얻어진 추출물을 EtOAc, n-BuOH 및 $H_2O$로 용매 분획하였다. 이중 EtOAc 분획으로부터 silica gel과 ODS column chromatography로 정제하여 5개의 화합물을 분리하였다. 각 화합물의 화학구조는 NMR, MS 및 IR 등의 스펙트럼 데이터를 해석하여, friedelin (1), ${\beta}$-amyrin (2), ${\beta}$-amyrin acetate (3), camphanediol (4), hispidulin (5)으로 동정하였다. 이 화합물들은 싸주아리쑥에서는 처음 분리되었다.

Metabolomic understanding of intrinsic physiology in Panax ginseng during whole growing seasons

  • Lee, Hyo-Jung;Jeong, Jaesik;Alves, Alexessander Couto;Han, Sung-Tai;In, Gyo;Kim, Eun-Hee;Jeong, Woo-Sik;Hong, Young-Shick
    • Journal of Ginseng Research
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    • 제43권4호
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    • pp.654-665
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    • 2019
  • Background: Panax ginseng Meyer has widely been used as a traditional herbal medicine because of its diverse health benefits. Amounts of ginseng compounds, mainly ginsenosides, vary according to seasons, varieties, geographical regions, and age of ginseng plants. However, no study has comprehensively determined perturbations of various metabolites in ginseng plants including roots and leaves as they grow. Methods: Nuclear magnetic resonance ($^1H$ NMR)-based metabolomics was applied to better understand the metabolic physiology of ginseng plants and their association with climate through global profiling of ginseng metabolites in roots and leaves during whole growing periods. Results: The results revealed that all metabolites including carbohydrates, amino acids, organic acids, and ginsenosides in ginseng roots and leaves were clearly dependent on growing seasons from March to October. In particular, ginsenosides, arginine, sterols, fatty acids, and uracil diphosphate glucose-sugars were markedly synthesized from March until May, together with accelerated sucrose catabolism, possibly associated with climatic changes such as sun exposure time and rainfall. Conclusion: This study highlights the intrinsic metabolic characteristics of ginseng plants and their associations with climate changes during their growth. It provides important information not only for better understanding of the metabolic phenotype of ginseng but also for quality improvement of ginseng through modification of cultivation.

분지형 폴리카보네이트의 분자량 조절 및 유변학적 특성 연구 (A Study on the Molecular Weight Control and Rheological Properties of Branched Polycarbonate)

  • 이봄이;프러산터;김희승;유승윤;김연철
    • 공업화학
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    • 제23권4호
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    • pp.388-393
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    • 2012
  • 말단캡핑제(end capping agent) 4종류와 함량별로 분지형 폴리카보네이트를 용융중합법으로 제조하였다. 합성된 분지형 폴리카보네이트의 화학구조는 FT-IR과 $^{1}H-NMR$ 스펙트럼을 이용하여 확인하였으며, 말단캡핑제의 반응여부는 FT-IR 스펙트럼의 수산기($3500\;cm^{-1}$) 존재여부로 확인하였다. 평균 분자량 및 분자량 분포도, 유리전이 온도 및 분해온도는 GPC, DSC와 TGA를 이용하여 측정하였다. 말단캡핑제의 화학구조에 따라 평균 분자량이 증가 또는 감소를 나타내었으며, 말단캡핑제로 4-tert-butylphenol (TBP)이 사용되었을 때 최적의 분자량 조절 결과를 나타내었다. 말단캡핑제의 함량이 증가할수록 평균분자량은 감소하였고, 4-tert-butylphenol이 0.05 mol%가 첨가될 때 폴리카보네이트의 대형 사출물 가공에 적합한 20000 정도의 수평균분자량을 나타내었다. 분지형 폴리카보네이트의 용융점도는 분자량이 감소할수록 감소하였으며, shear thinning effect에는 큰 영향을 주지 않음을 확인하였다.

춘란(Cymbidiym goeringii REICHB. fil)의 메탄올 추출물로부터 Sterol 화합물의 분리 (Isolation of Sterols from the Methanol Extracts of Cymbidium goeringii REICHB. fil)

  • 이진희;김동현;방면호;양혜정;방성훈;정인식;권병목;김성훈;김대근;박미현;백남인
    • Applied Biological Chemistry
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    • 제48권3호
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    • pp.263-266
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    • 2005
  • 춘란을 80% MeOH로 추출하고, 얻어진 추출물을 EtOAc, n-BuOH 및 $H_2O$로 용매 분획하였다. EtOAc 분획에 대하여 column chromatography를 반복하여 3종의 sterol을 분리하였다. 각각에 대하여 2D-NMR을 포함한 스펙트럼 데이터의 해석과 문헌 자료를 조사하여 ${\beta}-sitosterol$, daucosterol, ergosterol peroxide로 구조를 결정하였다. 이 화합물들은 춘란에서 이번에 처음 분리, 보고되었다.

The Preliminary Study on the Structure of Cop Protein by CD and NMR

  • Kim, Yun-Kyong;Park, Sang-Ho;Lee, Jee-Hyun;Kwak, Jin-Hwan;Lee, Bong-Jin
    • 한국자기공명학회논문지
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    • 제3권2호
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    • pp.100-108
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    • 1999
  • Cop protein is the transcription repressor protein in rolling circle replication plasmid. With antisense RNA, Cop protein controls the copy number of plasmid. Cop family proteins have been found in various plasmids. Among Cop family proteins, Cop studied in this paper consists of 55 amino acids (Mw. 6,400), and was known to have trimer structure. Since no structural facts are elucidated, we have carried out preliminary experiments aimed at the elucidation of its three dimensional structure. The secondary structure of Cop is studied by CD and NMR. To solve the aggregation of Cop at high concentration, we tested various detergents and salts. The addition of detergents and salts could not solve the aggregation problem. However, we found that concentration is important in solving the aggregation problem. We knew that 0.18mM in 50mM potassium phosphate without any other ingredients is maximum concentration not to aggregate. Wa also investigated the pH dependence of Cop protein, and knew that Cop protein is more stable in acid state. At various temperatures, 15N-1H HSQC spectra were measured in order to find the optimal experimental condition. To enhance the peak resolution, 3D NOESY-HSQC spectrum is acquired. Since there are NOE peaks in the NH-NH region, we knew that Cop protein has $\alpha$-helical content, which was also confirmed by CD.

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