• Title/Summary/Keyword: FT-NMR

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Solid-state Chracterization of the HIV Protease Inhibitor

  • Kim, Yong-Ae;Kim, Ae-Ri
    • Bulletin of the Korean Chemical Society
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    • v.23 no.12
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    • pp.1729-1732
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    • 2002
  • The LB71350,(3S, 4R)-Epoxy-(5S)-[[N-(1-methylethoxy)carbonyl]-3-(methylsulfonyl)-L-valinyl]amino]-N-[2-methyl-(1R)-[(phenyl)carbonylpropyl-6-phenylhexanamide, is a novel HIV protease inhibitor. Its equilibrium solubility at room temperature was less than $40{\mu}g/mL.$ It was speculated that the low aqueous solubility might be due to the high crystalline lattice energy resulting from intermolecular hydrogen bonds. The present study was carried out to learn the solid-state characteristics of LB71350 using analytical methods such as NMR, FT-IR and XRD. $^{13}C$ Solid-state NMR, solution NMR, and FT-IR spectra of the various solid forms of LB71350 were used to identify the conformation and structure of the solid forms. The chemical shifts of $^{13}C$ solid-state NMR spectra suggest that the crystalline form might have 3 intermolecular hydrogen bondings between monomers.

Characterization and Synthesis of Titanium (IV) Isopropoxide Derivatives (Titanium(IV) isoproxide 유도체의 합성 및 특성연구)

  • Jung, Mie-Won
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.509-514
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    • 1999
  • The systematic modification of titanium(IV) isopropoxide with acetic acid as a organic additive was done and identifided by FT-IR, $^1H$, $^{13}C$ NMR and UV-Vis spectroscopy. The structure was cbanged after hydrolysis-condensation reaction and drying process. The hydrolysis-condensation rates of modified Ti alkoxide with acetic acid were investigated by $^1H$ NMR spectroscopy. This modified Ti(IV) alkoxide was less reactive toward hydrolysis-condensation reaction than $Ti(OPr^i)_4$, which can be attributed to the stable ligand structure between Ti alkoxide and ligand. The structural change on obtained from gel powders with heat treatment was also observed by FT-IR spectroscopy.

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Pharmaceutical Application of FT-NMR (FT-NMR의 약학적(藥學的) 응용(應用))

  • Yu, Byung-Sul
    • Korean Journal of Pharmacognosy
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    • v.9 no.1
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    • pp.1-9
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    • 1978
  • The principle of Fourier Transform Nuclear Magnetic Resonance and its usefulness in the fields of pharmacy and biological sciences are described. 1. The $^1H\;and\;^{13}C$ NMR spectra of triostin A and its mixture with purine derivatives were taken. From the analysis of the spectra it has established that triostin A, which exists in two symmetric conformers in chloroform solution, forms complexes only with purine derivatives by the participation of one of the conformers. 2. Also, the $^{13}C$ NMR spectra of "intact" substances in the field of pharmacognosy were taken. From the spectra it was suggested that the method is very useful for natural product research in cooperation with the chemical method.

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Vinyl Addition Copolymerization of Norbornene/5-Vinyl-2-norbornene with Cationic $\eta^{3_}$-Allyl Palladium Catalyst and Their Post-Reaction (양이온성 $\eta^{3_}$알릴 팔라듐 촉매를 사용한 노보넨/5-비닐-2-노보넨의 비닐 부가 공중합과 이를 이용한 고분자 후반응)

  • 안재철;박수현;이광희;박기홍
    • Polymer(Korea)
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    • v.27 no.5
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    • pp.429-435
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    • 2003
  • Vinyl addition copolymerizations of norbornene (NB) and 5-vinyl-2-norbomene (VNB) were carried out using a cationic η$^3$-allyl palladium catalyst in the various mole ratio of comonomers. The copolymers could be obtained in good yield (65∼85%) with high weight-average molecular weights (M$_{w}$ > 760,000). Depending on increasing VNB contents, the molecular weight and yield of the copolymers decreased. FT-IR analysis confirmed that actual contents of VNB in polymer were proportional to the feeding content of VNB. From $^1$H-NMR spectroscopy, we found that both exo and endo VNB isomer were copolymerized with NB. Thermal stabilities of NB-VNB copolymers were independent on the VNB content and their initial decomposition temperatures were about 300 C. The NB-VNB copolymers were followed by epoxidation by using m-CPBA and hydroxylation by 9-BBN, respectively, and these post-polymers were characterized by FT-IR spectroscopy and $^1$H-NMR analysis..

Phosphorylation of silk fibroin and its properties (견 피브로인의 인산화와 그 특성)

  • 문장희;김정호;배도규;신봉섭
    • Journal of Sericultural and Entomological Science
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    • v.43 no.2
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    • pp.116-124
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    • 2001
  • To improve the functional properties as a food, silk fibroin was phosphorylated with STMP In the phosphorylation reaction of silk fibroin, the degree of phosphorylation was increased with high alkali index and treatment temperature. Depending on treatment time and concentration of STMP it was rapidly increased up to 1hr. and 50%, but slowly above that time and 100%. It was indicated in the results of FT-IR analysis and $\^$31/p NMR spectroscopy of phosphorylated fibroin that it had a close ∝-helix and poly-phosphate structure. The more phosphorylation of fibroin made more turbidity, foam expansion and foam stability, but less solubility. Emulsifying activity was increased up to P100, but slightly decreased above Pl00 and emulsifying stability was constantly increased on the progressing of phosphorylation.

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Property Change of Solution by Pulsed Electric Field Treatment (펄스 전기장 처리에 의한 수용액의 물성 변화)

  • Choi, Seung-pil;Kim, Chan-Soo;Kim, Jong-Oh
    • Journal of the Korean GEO-environmental Society
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    • v.12 no.9
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    • pp.63-69
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    • 2011
  • The objective of this study is to investigate the change of physicochemical properties of humic acid, surfactants and water by pulsed electric field treatment. Critical micelle concentration(CMC) of surfactants and physicochemical properties of water were determined by the conductivity measurement, FT-IR and NMR, respectively. In electric field processing, structural changes of C-N complex and C=O were founded by FT-IR analysis. The increase of Hertz wave was in the range of 2.3 to 9.9 Hz in NMR analysis. CMC of cation and anion surfactant decreased to 1.3% and 9.2%, respectively, while the value of UV-vis increased. UV-vis of humic acid decreased by pulsed electric field. Therefore, application of pulsed electric field systeme was directly indicated to influence the physicochemical properties of water and organic compounds.

Preparation and Characterization of La0.8Ca0.2MnO3 (La0.8Ca0.2MnO3의 합성 및 특성연구)

  • 정미원;이지윤;김현정
    • Journal of the Korean Ceramic Society
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    • v.40 no.5
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    • pp.434-440
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    • 2003
  • The powders of L $a_{0.8}$C $a_{0.2}$Mn $O_3$ Colossal Magnetoresistance (CMR) materials were synthesized by sol-gel process. Lanthanum(H), Calcium(II) and Manganese(III) 2,4-Pentanedionate were dissolved in a mixed binary solution consisted of propionic acid and methanol with PEG (15 wt%) aqueous solution. The progress of reactions was monitored by FT-IR spectroscopy. The Lao scao.2Mn03 gel powders were annealed at various temperatures. The structural changes were investigated by FT-IR, CP/MAS $^{ 13}$C solid state NMR spectroscopy and XRD. The thermochemical property, particle characterization, microstructure of sintered sample, and cation composition of gel powder were studied by TG/DTA, FE-SEM and ICP-AES. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

Studies on the Oxidative Structural Change of Azo Dye Acid Red 27 by Ozone (O3에 의한 아조염료 Acid Red 27의 산화분해시 구조 변화에 관한 연구)

  • Baek, Mi-Hwa;Kim, Dong-Su
    • Journal of Korean Society on Water Environment
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    • v.21 no.6
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    • pp.564-568
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    • 2005
  • The structural change of azo dye (Acid Red 27) by oxidation with ozone has been investigated using FT-IR and $^1H$ NMR. The solution pH was observed to decrease during oxidation reaction, which was considered to be due to the generation of several organic and inorganic acids as the result of the decomposition of azo compound. The FT-IR analysis showed that changes of specific absorption bands of Acid Red 27 were observed after ozonation. When azo dye was oxidized by ozone, several new peaks were shown to appear by $^1H$ NMR analysis and the peaks were generally shifted to the direction of up field. This was presumably due to the breakage of benzene ring contained in the molecular structure of Acid Red 27 by the oxidation and the shape of peaks was shown to change according to the reaction time.

Structure and Hydrolysis Study of Inclusion Complex of Cyclodextrin and Aspirin (시클로덱스트린과 아스피린의 포접화합물의 구조와 가수분해에 관한 연구)

  • 최희숙;김경순
    • Journal of Life Science
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    • v.10 no.1
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    • pp.86-93
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    • 2000
  • Specific molecular recognition of cyclodextrin and aspirin was determined. A stable 1:1 inclusion complex was established in solution. The distinct structure of inclusion complex was elucidated by FT-IR, FAB-MS, UV, 1H NMR, and 13C NMR spectroscopy. Based on the 1H NMR data, a time-averaged conformation of $\alpha$-cyclodextrin exhibited significant catalytic activity toward the hydrolysis of aspirin in alkaline solution.

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