• Natural Product Sciences
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• 제6권2호
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• pp.66-69
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• 2000

Salvia bucharica belonging to the family Lamiaceae (Labiatae), afforded a novel terpenoid (1) named as salvatrione. The structure of 1 was elucidated through extensive 2-D NMR experiments and the biogenetic pathway of 1 has also been proposed. On biogenetic grounds, 1 may be considered to be a pseudo-triterpenoid as it is derived from the coupling of mono/ diterpenic units and not from squalene.

• Bulletin of the Korean Chemical Society
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• 제23권1호
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• pp.35-40
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• 2002

Photoreaction of guest organic anions in layered organic-inorganic hybrid materials was investigated. The layered hybrids were synthesized by an anion-exchange reaction of $[LiAl_2(OH)_6]Cl{\cdot}yH_2O$ layered double hydroxide with aqueous (Z,Z)- and (E,E)-muconates under inert atmospheric condition, to give new organicinorganic hybrids of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$ and $[LiAl_2(OH)_6]_2[(E,E)-C_6H_4O_4]{\cdot}H_2O$, respectively. The basal spacings calculated by XRPD of intercalates indicate that muconate anions have almost vertical arrangements against the host $[LiAl_2(OH)_6]^+$ lattices in the interlayer of organic-inorganic hybrid materials. When UV light was irradiated on the suspension of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$, the (Z,Z)-muconate anions of the gallery space of hybrids were polymerized in the aqueous media while it was isomerized into more stable (E,E)-muconate in the methanollic suspension in the presence of catalytic amount of molecular iodine. All the products were characterized using elemental analysis, TGA, XRPD, FT-IR, $^1H$ NMR and $^{13}C$ CP-MAS NMR.

• Bulletin of the Korean Chemical Society
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• 제30권8호
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• pp.1715-1718
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• 2009

A series of sitting-atop (SAT) complexes, [(ZrO)$H_2t(X)pp(NO_3)_2$], have been prepared via the reactions of free base meso-tetraarylporphyrins, $H_2$t(X)pp, with zirconyl nitrate hydrate, ZrO(N$O_3)_2{\cdot}xH_2$O. The products have been characterized by a variety of methods including $^1H\;NMR,\;^{13}C$ NMR, IR and UV-Vis spectroscopies, elemental analysis and conductance measurements. The data indicate that the meso-tetraarylporphyrins coordinate with two pyrrolenine nitrogen atoms to the zirconyl cation located above the distorted porphyrin plane and two protons remain on the pyrrole nitrogens. Such half sandwich-type sitting-atop complexes may be considered as models for the initial steps of the metallation of the macrocycles.

• Bulletin of the Korean Chemical Society
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• 제31권4호
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• pp.934-940
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• 2010

The reduction of [$Os_3(CO)_{11}P(OMe)_3$] and subsequent ionic coupling of the reduced species with $[Ru({\eta}^5-C_5H_5)(CH_3CN)_3]^+$ resulted in the formation of [$Os_3(CO)_{11}P(OMe)_3(Ru({\eta}^5-C_5H_5))_2$] which can be converted to spiked tetrahedral cluster, [$HOs_3(CO)_{11}P(OMe)_3Ru_2({\eta}^5-C_5H_5)(C_5H_4)$] via the intramolecular hydrogen transfer. Due to the unavailability of a suitable single crystal, the PW91/SDD and LDA/SDD density functional methods were used to predict possible structures and the available spectroscopic information (IR, NMR) of [$Os_3(CO)_{11}P(OMe)_3(Ru({\eta}^5-C_5H_5))_2$]. The most probable geometry found by constrained search is the isomer (a2) in which the phosphite, $P(OMe)_3$, occupies an axial position on one of the two osmium atoms that is edge bridged by the $Ru(CO)_2({\eta}^5-C_5H_5)$ unit. By using the most probably geometry, the predicted infrared frequencies and $^1H$, $^{13}C$ and $^{31}P$ NMR chemical shifts of the compound are in the same range as the experimental values. For this type of complex, the LDA/SDD method is appropriate for IR predictions whereas the OPBE/IGLO-II method is appropriate for NMR predictions. The activation energy and reaction energy of the intramolecular hydrogen transfer coupled with the structural change of the transition metal framework were estimated at the PW91/SDD level to be 110.32 and -0.14 kcal/mol respectively.

• Journal of Ginseng Research
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• 제38권2호
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• pp.116-122
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• 2014

Ginseng roots were extracted with aqueous methanol, and extracts were suspended in water and extracted successively with ethyl acetate and n-butanol. Column chromatography using the n-butanol fraction yielded four purified triol ginseng saponins: the ginsenosides Re, Rf, Rg2, and 20-gluco-Rf. The physicochemical, spectroscopic, and chromatographic characteristics of the ginsenosides were measured and compared with reports from the literature. For spectroscopic analysis, two-dimensional nuclear magnetic resonance (NMR) methods such as $^1H$-$^1H$ correlation spectroscopy, nuclear Overhauser effect spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond connectivity were employed to identify exact peak assignments. Some peak assignments for previously published $^1H$-and $^{13}C$-NMR spectra were found to be inaccurate. This study reports the complete NMR assignment of 20-gluco-Rf for the first time.

• BMB Reports
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• 제34권5호
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• pp.446-451
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• 2001

The interaction of cytochrome c with binary phospholipid mixtures was investigated by solid-state $^2H$- and $^{31}P$-NMR. To examine the effect of the interaction on the glycerol backbones, the glycerol moieties of phosphatidylcholine (PC), and cardioliph (CL) were specifically deuterated. On the binding of cytochrome c to the binary mixed bilayers, no changes in the quadrupole splittings of each of the components were observed for the PC/PG, PE/CL and PE/PG liposomes. In contrast, the splittings of CL decreased on binging of protein to the PC/CL liposomes, although those of PC did not change at all. This showed that cytochrome c specifically interacts with CL in PC/CL bilayers, and penetrates into the lipid bilayer to some extent so as to perturb the dynamic structure of the glycerol backbone. This is distinctly different from the mode of interaction of cytochrome c with other binary mixed bilayers. In the $^{31}P$-NMR spectra, line broadening and a decrease of the chemical shift anisotropy were observed on the binding of cytochrome c for all binary mixed bilayers that were examined. These changes were more significant for the PC/CL bilayers. Furthermore, the line broadening is more significant for PC than for CL in PC/CL bilayers. Therefore, it can be concluded that with the polar head groups, not only CL but also PC are involved in the interaction with cytochrome c.

• Bulletin of the Korean Chemical Society
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• 제31권4호
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• pp.984-988
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• 2010

1-(Fluoren-2-yl)-benzo[d][1,2,3]triazoles 5a-b were synthesized starting from 2-nitrofluorene. 2-Nitrofluorenes 1a-b were reduced by catalytic hydrogenation, reacted with 2,4-dinitrofluorobenzene followed by catalytic hydrogenation to afford 2-(N-2,4-diaminophenyl)aminofluorenes 4a-b. Diazotization of 4a-b with $NaNO_2/H_2SO_4$ followed by treatment with $H_3PO_2$ gave 5a-b. Sulfonation of 5a-b yielded 7-benzotriazol-1-yl-fluorene-2-sulfonic acids 6a-b. The structures of 5b and 6b were firmly identified by X-ray crystal analysis in addition to $^1H$ NMR, $^{13}C$ NMR, and elemental analysis.

• 대한화학회지
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• 제39권11호
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• pp.856-862
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• 1995

본 연구의 텅스텐 옥소-니트로실 착물 $(n-Bu_4N)_2[W_5O_{12}(NO)_2{RC(NH_2)NHO}_2{RC(NH)NO}_2]{R\;=\;(CH_3)CH, CH_3CH_2CH_2,CH_3SCH_2}$은 텅스텐(VI) 다핵 착물 $(n-Bu_4N)_2[W_6O_{19}]$, 텅스텐 디니트로실 단핵 착물 $[W(NO)_2(acac)(CH_3CN)_2](BF_4)$ 및 부틸 아미드옥심 유도체의 반응에서 얻었다. 합성한 착물은 원소분석, 적외선, 전자 흡수 및 핵자기 공명 스펙트럼에 의해 특성을 조사하였다. 전자를 끌어당기는 ${W(NO)_2}^{2+}$ 단위체는 두 개의 이핵체 ${W_2O_5}^{2+}$ 사이의 중심에 삽입되어 오핵종을 이룬다. $(n-Bu_4N)_2[W_5O_{12}(NO)_2{(CH_3)_2CHC(NH_2)NHO}_2/{(CH_3)_2/CHC(NH)NO}_2]$의 $^1{H} NMR$ 스펙트럼에서 네 개의 이중선이 나타남으로 양성자간의 상호작용이 큰 것을 추정할수있다. $^{13}C$ NMR 스펙트럼은 배위된 네 개의 배위자중 두개의 배위자가 나타남으로 두 배위자의 서로 다른 배위모형과 대칭성에 대한 정보를 준다. ${W(NO_2)}^{2+}$ 단위체는 형식상 시스형이며 기하학적으로 $C_{2v}$ 대칭을 가진다.

• 한국자기공명학회논문지
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• 제14권2호
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• pp.117-126
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• 2010

Hsp33 is a molecular chaperone achieving a holdase activity upon response to a dual stress by heat and oxidation. Despite several crystal structures available, the activation process is not clearly understood, because the structure inactive Hsp33 as its reduced, zinc-bound, monomeric form has not been solved yet. Thus, we initiated structural investigation of the reduced Hsp33 monomer by NMR. In this study, to overcome the high molecular weight (33 kDa), the protein was triply isotope-[$^{13}C$, $^{15}N$, $^2H$]-labeled and its inactive, monomeric state was ensured. 2D-[$^1H$, $^{15}N$]-TROSY and a series of triple resonance spectra could be successfully obtained on a high-field (900 MHz) NMR machine with a cryoprobe. However, under all of the different conditions tested, the number of resonances observed was significantly less than that expected from the amino acid sequence. Thus, a possible contribution of dynamic conformational exchange leading to a line broadening is suggested that might be important for activation process of Hsp33.

• 대한화학회지
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• 제39권4호
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• pp.301-305
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• 1995

인도네시아 Manado만의 Sulawesi에서 채집한 해면 Spongia sp.로부터 KB Cancer cell line에 대하여 활성을 갖는 halenaquinone, epispongiatriol 및 aldisin을 분리하였다. 이들의 구조를 $1^H,\;13^C\;NMR\;1^H\;13^C(1\;bond)$ Heteronuclear Multiple Quantum Coherence Spectroscopy (HMQC), 1H 13C(2 and 3 bond) Heteronuclear Multiple Bond Correlation Spectroscopy (HMBC), Electron Impact Mass Spectroscopy (EI ms) 및 IR로 밝혔다.