• 제목/요약/키워드: 1H-NMR spectroscopy

검색결과 577건 처리시간 0.028초

6,7-Dibromo-1,4-dihydropentiptycene-1,4-epoxide의 합성 (Synthesis of 6,7-Dibromo-1,4-dihydropentiptycene-1,4-epoxide)

  • 양진석;엄성용;박철영
    • 통합자연과학논문집
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    • 제3권2호
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    • pp.103-106
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    • 2010
  • Pentiptycene and its derivatives having cavity, ${\pi}-{\pi}$ stacking prohibition, and AIEE functionalities were synthesized. 6,7-Dibromo-1,4-dihydropentiptycene-1,4-epoxide was obtained from the reaction of 6,7-dibromo-1,4-dihydronaphthalene-1,4-epoxide and anthracene. All the synthesized compounds were characterized by fourier transform infrared spectroscopy (FTIR), 1H-NMR, and 13C-NMR spectroscopy. Prepared pentiptycene derivatives could be useful precursor for organofluorene compounds which could be an excellent candidate for electronic devices such as organic light-emitting diodes (OLED's) and chemical sensor.

Solution and Solid-state Vanadium-51 NMR Studies of Vanadium (V) Complexes

  • Lee, Man-Ho
    • 한국자기공명학회논문지
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    • 제1권1호
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    • pp.1-6
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    • 1997
  • Several dioxovanadate (V) complexes are synthesized and studied by solution and solid-state 51V NMR spectroscopy. In the results, large 51V chemical shift anisotropy ({{{{ DELTA delta }}a = -800 ∼720 ppm) and quadrupole coupling (e2q /h = 7.50 ∼ 9.16 MHz) were observed in the solid-state complexes. The isotropic chemical shifts of the solid samples are very close to the values obtained from solution measurements.

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Constructing Overhauser Dynamic Nuclear Polarization-Nuclear Magnetic Resonance System Using Benchtop Electron Paramagnetic Resonance Spectrometer

  • Saun, Seung-Bo;Kim, JiWon;Han, Oc Hee
    • 한국자기공명학회논문지
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    • 제22권2호
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    • pp.34-39
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    • 2018
  • The Nuclear Magnetic Resonance (NMR) technique using Dynamic Nuclear Polarization (DNP) procedures is one of the promising techniques that enable overcoming low sensitivity problems in NMR spectroscopy. We constructed an ODNP-NMR system using a commercial benchtop EPR spectrometer. The $^1H$ NMR peak area of water in aqueous solutions of 4-hydroxy-TEMPO was enhanced more than 95 times in the ODNP-NMR experiments. Our signal enhancement results were about 55% of the previously reported result. This could be due to non-uniform microwave power over a sample and unwanted sample heating by microwave. However, this portable ODNP-NMR spectrometer will be eventually useful for site-specific detection with nano-scale spatial resolutions and molecular dynamics studies with significantly improved signal sensitivity.

에스테르기를 도입한 술폰화 프탈계 폴리이미드와 나프탈렌계 폴리이미드의 수화안정성에 관한 연구 (Hydrolysis Stability of Sulfonated Phthalic and Naphthalenic Polyimide with Ester Bond)

  • 이영무;이창현;손준용;박호범
    • 멤브레인
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    • 제13권2호
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    • pp.110-117
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    • 2003
  • 술폰화 폴리이미드는 클로로알칼리 전기분해, 양이온교환수지 및 연료전지용 고분자진해질막 등과 같은 많은 응용에 있어 유용한 재료로서 연구되어지고 있다. 그러나, 이러한 응용이 이루어지는 과정에 있어서 시간에 따라 연속적인 탈수공정이나 고분자의 분해에 따른 성능 감소 등이 보고되었다. 술폰화 고분자 분해의 주요 원인 중 하나로서 고분자 분자량의 감소 및 고분자 사슬의 절단으로 이끌어지는 가수분해를 들 수 있다. 따라서, 본 연구의 목적은 수화조건 하에서의 $-SO_3$H와 연결된 이미드 사이클과 부가적인 에스테르 결합의 분해를 조사하는 데 있다. 사슬의 분리에 대해 가능한 정확한 정보를 얻고 이를 확인하기 위해서는 $^1H$$^{13}C$ NMR, FT-IR 분석을 이용했으며, 또한 보다 편리한 분석을 위해서 model compound를 사용하여 실험을 수행하였다. 결과적으로, 술폰화 폴리이미드의 수화안정성을 평가하기 위해서 프탈계 및 나프탈렌계 이미드 고리와 에스테르 결합을 갖는 model compound를 합성하였고, 제조된 model compound를 이용하여 $80^{\circ}C$ 초순수 하에서 aging 실험을 수행하였고, lyophilization technique을 사용하여 반응을 중지시켰다. Aging된 product는 NMR, FT-IR spectroscopy를 이용하여 분석하였다.

Electron Withdrawing Group을 함유한 Polythiophene의 합성과 특성에 관한 연구 (Synthesis and Characteristic of Polythiophene Containing Electron Withdrawing Group)

  • 홍혁진;한신호
    • 공업화학
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    • 제23권6호
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    • pp.539-545
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    • 2012
  • 전자를 끌어당기는 benzotriazole을 vinylene으로 thiophene과 연결한 3-(2-benzo-triazolovinyl)thiophene (BVT)을 합성하고, FT-IR 및 $^1H$-NMR, $^{13}C$-NMR, 2D hetero-cosy spectra로 구조분석을 하였다. 합성한 BVT와 3-octylthiophene (OT)을 공중합 하였다. 공중합체들은 수평균 분자량 12000 (PDI 2.67)과 15000 (PDI 2.55)을 나타내었으며, THF, TCE와 chloroform 등의 유기용매에 잘 용해되었다. 공중합체들의 BVT와 OT의 공중합된 비율은 $^1H$-NMR spectra에 의하여 BVT : OT = 1 : 1.8과 1 : 2.8 (mol/mol)로 확인되었다. 파장 470 nm와 465 nm에서 UV-vis 최대 흡수를 나타내었고, photoluminescence (PL)는 각각 ${\lambda}_{max}$ = 662 nm와 641 nm로 나타나 적색계로 관찰되었다. 공중합체의 band gap은 각각 1.96 eV, 2.02 eV로 poly(3-octylthiophene)보다 더 증가하였다. 또한, poly(3-octylthiophene)에 비해서 HOMO 에너지 준위는 모두 낮아졌으나, LUMO 에너지 준위는 모두 높아졌다.

$^1H$-NMR에 의한 Xylan의 황산가수분해 과정에서 나타나는 반응 동력학 연구 (Kinetic Study of Xylan Hydrolysis and Decomposition in Concentrated Sulfuric Acid Hydrolysis Process by $^1H$-NMR Spectroscopy)

  • 조대행;김용환;김병로;박종문;성용주;신수정
    • 펄프종이기술
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    • 제43권3호
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    • pp.52-58
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    • 2011
  • Proton-NMR spectroscopic method was applied to kinetic study of concentrated sulfuric acid hydrolysis reaction, especially focused on 2nd step of acid hydrolysis with deferent reaction time and temperature as main variables. Commercial xylan extracted from beech wood was used as model compound. In concentrated acid hydrolysis, xylan was converted to xylose, which is unstable in 2nd hydrolysis condition, which decomposed to furfural or other reaction products. Without neutralization steps, proton-NMR spectroscopic analysis method was valid for analysis of not only monosaccharide (xylose) but also other reaction products (furfural and formic acid) in acid hydrolyzates from concentrated acid hydrolysis of xylan, which was the main advantages of this analytical method. Higher temperature and longer reaction time at 2nd step acid hydrolysis led to less xylose concentration in xylan acid hydrolyzate, especially at $120^{\circ}C$ and 120 min, which meant hydrolyzed xylose was converted to furfural or other reaction products. Loss of xylose was not match with furfural formation, which meant part of furfural was degraded to other undetected compounds. Formation of formic acid was unexpected from acidic dehydration of pentose, which might come from the glucuronic acid at the side chain of xylan.

Synthesis and Characterization of Novel pH-Sensitive Hydrogels Containing Ibuprofen Pen dents for Colon-Specific Drug Delivery

  • Mahkam, Mehrdad;Poorgholy, Nahid;Vakhshouri, Laleh
    • Macromolecular Research
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    • 제17권9호
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    • pp.709-713
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    • 2009
  • The aim of this study was to develop novel intestinal specific drug delivery systems with pH sensitive swelling and drug release properties. The carboxyl group of ibuprofen was converted to a vinyl ester group by reacting ibuprofen and vinyl acetate as an acylating agent in the presence of catalyst. The glucose-6-acrylate-1, 2, 3, 4-tetraacetate (GATA) monomer was prepared under mild conditions. Cubane-1, 4-dicarboxylic acid (CDA) linked to two 2-hydroxyethyl methacrylate (HEMA) group was used as the crosslinking agent (CA). Methacrylic-type polymeric prodrugs were synthesized by the free radical copolymerization of methacrylic acid, vinyl ester derivative of ibuprofen (VIP) and GATA in the presence of cubane cross linking agent. The structure of VIP was characterized and confirmed by FTIR, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The composition of the cross-linked three-dimensional polymers was determined by FTIR spectroscopy. The hydrolysis of drug polymer conjugates was carried out in cel-lophane membrane dialysis bags, and the in vitro release profiles were established separately in enzyme-free simulated gastric and intestinal fluids (SGF, pH 1 and SIF, pH 7.4). The detection of a hydrolysis solution by UV spectroscopy at selected intervals showed that the drug can be released by hydrolysis of the ester bond between the drug and polymer backbone at a low rate. Drug release studies showed that increasing the MAA content in the copolymer enhances the rate of hydrolysis in SIP. These results suggest that these polymeric prodrugs can be useful for the release of ibuprofen in controlled release systems.

2차 아미노기가 결합된 실리카 나노 입자 표면에 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate의 마이클 부가 반응에 대한 분광학적 분석 (Spectroscopic Analysis on Michael Addition Reaction of Secondary Amino Groups on Silica Surface with 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate)

  • 이상미;하기룡
    • 폴리머
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    • 제38권2호
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    • pp.257-264
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    • 2014
  • 본 연구에서는 나노크기의 실리카 입자를 2차 아미노기를 가지는 dipodal 형태의 실란커플링제인 bis[3-(trimethoxysilyl)propyl]ethylenediamine(BTPED)으로 표면 개질한 후, 실리카에 도입되는 2차 아미노기인 N-H기와 마이클 부가 반응이 가능한 acrylate기를 가지는 3-(acryloyloxy)-2-hydroxypropyl methacrylate(AHM)로 표면 처리를 하여 중합 반응성 methacrylate기를 도입하는 연구를 수행하였다. 1 분자에 2차 아미노기를 2개 가지는 BTPED와 마이클 부가 반응성이 있는 acrylate기와 부가 반응성이 없는 methacrylate기를 각각 1개씩 가지는 AHM을 사용하여 BTPED와 AHM의 투입량 및 개질 반응 시간의 변화가 실리카 표면의 methacrylate기 도입에 미치는 영향을 Fourier transform infrared spectroscopy(FTIR), elemental analysis(EA)와 액체 및 고체 상태 cross polarization magic angle spinning(CP/MAS) nuclear magnetic resonance spectroscopy(NMR)법을 사용하여 분석하였다. 실리카 표면에 BTPED 를 도입하는 반응은 1시간 내에, BTPED로 개질된 실리카의 N-H기에 대한 AHM의 acrylate기와의 마이클 부가 반응에 따른 methacrylate기 도입은 2시간 내에 반응이 각각 완결됨을 확인하였다. 또한 BTPED로 개질된 실리카에 대하여 투입되는 AHM의 몰 비가 증가할수록 N-H기와 acrylate기의 마이클 부가 반응으로 인한 methacrylate기의 도입이 증가하였으며 이는 AHM을 도입했을 때 나타나는 FTIR 스펙트럼의 C=O 피크 면적 변화로 확인하였다. 위의 결과를 EA 및 고체 상태 $^{13}C$$^{29}Si$ NMR 분석으로도 확인하였다.

피페리딘 디티오카바메이트의 구리(II)의 착물합성과 분석적 응용 (Synthesis and Analytical Application of Piperidine Dithiocarbamate Complex of Copper(II))

  • 김찬우;김창수
    • 분석과학
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    • 제12권1호
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    • pp.1-6
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    • 1999
  • 구리(II)이온과 피페리딘 디티오카바메이트(Pipdtc)의 반응에서[$Cu(Pipdtc)_2$]를 합성하였다. 이 착물은 디메틸포름아미드, 디메틸술폭시드의 극성 유기용매에 잘 녹는다. 원소분석, 몰전도도, 적외선 흡수스펙트럼, 전자흡수스펙트럼 및 핵자기공명스펙트럼에서 부터 평면 사각형의 구조를 가짐을 알 수 있었다. 수용액에서 부터 사염화탄소에 의한 Cu(II)-Pipdtc착물의 추출은 pH가 6.0~10범위에서 이루어졌다. 구리(II)의 피페리딘 디티오카바메이트 용액은 pH 9.0에서 ${\sim}8.0{\times}10^{-5}M$까지 Beer의 법칙에 따랐다.

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Preparation of polymeric nanoparticles from hydrophobically modified pullulan for hydrophobic drug carrier

  • Kim, In-Sook;Kim, Sung-Ho
    • 대한약학회:학술대회논문집
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    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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    • pp.409.1-409.1
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    • 2002
  • For the development of a biocompatible nano-scale drug carrier. hydrophilic polysaccharide pullulan was hydrophobized by the conjugation with fatty acid. The synthesized polymers were characterized by the measurements of fourier transform infrared (FT -IR) spectroscopy and 1H -nuclear magnetic resonance (NMR) spectroscopy. In aqueous solution. hydrophobically modified puliulan was self-assembled and structured into the core-shell type nanoparticles. (omitted)

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