• 약학회지
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• 제39권6호
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• pp.600-609
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• 1995

Studies on the pharmaco-constituents from the leaves of Cercts chinensis which have been used for the treatment of inflammation, contusion, dilated blood, pain of heart and stomach, edema, etc. in Korean folk remedies were carried out. Dried leaves of the plant were extracted with MeOH. The MeOH extract was suspended in distilled water and subsequently fractionated with $Et_{2}O$ and n-BuOH. From the $Et_{2}O$ and n-BuOH fractions, six phenolic compounds were isolated and identified as myricitrin($C_{21}H_{20}O_{12}, {\;}m.p.{\;}199~200^{\circ}$. $4myricetin-3-O-{\alpha}-L-rhamnopyranoside$), kaempferol($C_{15}H_{10}O_{6}, {\;}m.p. 276^{\circ}$), quercetin($C_{15}Ha_{10}O_{7}, {\;}m.p.{\;}313~314^{\circ}$), quercitrin ($C_{21}H_{20}O_{12}, {\;}m.p.{\;}176~178^{\circ}, {\;}quercetin-3-O-{\alpha}-L-rhamnopyranoside$), gallicin ($C_{8}H_{8}O_{5}, {\;}m.p.{\;}202~203^{\circ}$. methyl gallate), gallic acid ($C_{7}H_{6}O_{5}, {\;}m.p.{\;}260~265^{\circ}) through their physico-chemical data and UV, IR, EI-MS, $^{13}C-NMR$, and $^{1}H-NMR$ analysis with authentics.

• Bulletin of the Korean Chemical Society
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• 제13권3호
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• pp.296-306
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• 1992

$^{13}C$ spin-lattice relaxation times were measured for n-alkanes of moderate chain length, ranging from n-octane to n-dodecane, under the condition of proton broad-band decoupling within the temperature range of 248-318 K in order to gain some insight into basic features of segmental motions occurring in long chain ploymeric molecules. The NOE data showed that except for methyl carbon-13 dipole-dipole interactions between $^{13}C$ and directly bonded $^1H$ provide the major relaxation pathway, and we have analyzed the observed $T_1data$ on the basis of the internal rotational diffusion theory by Wallach and the conformational jump theory by London and Avitabile. The results show that the internal rotational diffusion constants about C-C bonds in the alkane backbone are all within the range of $10^9\;-10^10\;sec^{-1}$ in magnitude while the mean lifetimes for rotational isomers are all of the order of $10^{-11}\;-10^{-10}$ sec. Analysis by the L-A theory predicts that activation energies for conformational interconversion between gauche and trans form gradually increase as we move from the chain end toward the central C-C bond and they are within the range of 2-4 kcal/mol for all the compounds investigated.

• Bulletin of the Korean Chemical Society
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• 제12권2호
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• pp.130-137
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• 1991

The following new cryptand 221 complexes of lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate have been synthesized: $(Ln(C_{16}H_{32}N_2O_5)(H_2O)_2(NO_3)_3\ and \((UO_2)_2(C_{16}H_{32}N_2O_5)(H_2O)_4(NO_3)_4$. These complexes have been identified by elemental analysis, moisture titration, conductivity measurements and various spectroscopic techniques. The proton and carbon-13 NMR as well as calorimetric measurements were used to study the interaction of cryptand 221 with La(Ⅲ), Pr(Ⅲ ), Ho(Ⅲ) and $UO_2(Ⅱ)$ ions in nonaqueous solvents. The bands of metal-oxygen atoms, metal-nitrogen atoms and O-U-O in the IR spectra shift upon complexation to lower frequencies, and the vibrational spectra ({\delta}NMN$) of metal-amide complexes in the crystalline state exhibit lattice vibrations below 300 $cm^{-1}$. The NMR spectra of the lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate complexes in nonaqueous solvents are quite different, indicating that the ligand exists in different conformation, and also the $^1H$ and $^{13}C-NMR$ studies indicated that the nitrogen atom of the ring has greater affinity to metal ions than does the oxygen atom, and the planalities of the ring are lost by complexation with metal ions. Calorimetric measurements show that cryptand 221 forms more stable complexes with $La^{3+}$ and $Pr^{3+}$ ions than with $UO^{22+}$ ion, and $La^{3+}/Pr^{3+}$ and $UO^{22+}/Pr^{3+}$ selectivity depends on the solvents. These changes on the stabilities are dependent on the basicity of the ligand and the size of the metal ions. The absorption band (230-260 nm) of the complex which arises from the direct interaction of macrocyclic donor atoms with the metal ion is due to n-{\delta}*$ transition and also that (640-675 nm) of $UO^{22+}$-cryptand 221 complex, which arises from interaction between two-dioxouranium(Ⅵ) ions in being out of cavity of the ligand ring is due to d-d* transition.

• 한국미생물·생명공학회지
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• 제25권5호
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• pp.483-489
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• 1997

Sulforhodamine B (SRB) and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) assay, RNA dot blot and Northern hybridization analysis were performed to screen microorganisms for the production of anticancer agent. Among microorganisms tested, strain YP-1 was selected for its cytotoxicity and ability to reduce the level of c-myc RNA. Strain YP-1 was identified as Streptomyces endus. The anticancer material produced by Streptomyces endus YP-1 was sequentially purified by solvent extraction, silica gel column chromatograpby, preparative TLC and preparative HPLC. The cancer material identified as azalomycin B by the instrumental analyses such as $^{1}$H-NMR, $^{13}$C-NMR, Mass, IR and UV absorption. It was colorless amorphous powder and its molecular weight was 1025.278. Azalomycin B, produced by Streptomyces endus YP-1, showed anticancer activity against several human cancer cell lines and reduction of c-Myc protein level in Colo320 DM cells which was determined by Western blot analysis.

• Bulletin of the Korean Chemical Society
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• 제31권12호
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• pp.3553-3560
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• 2010

A new hydrazone derivative compound has been synthesized and characterized by IR, $^1H$-NMR, $^{13}C$-NMR and UV-vis. spectroscopy techniques, elemental analysis and single-crystal X-ray diffraction (XRD). The new compound crystallizes in monoclinic space group C2/c. In addition to the crystal structure from X-ray experiment, the molecular geometry, vibrational frequencies and frontier molecular orbitals analysis of the title compound in the ground state have been calculated by using the HF/6-31G(d, p), B3LYP/6-311G(d, p) and B3LYP/6-31G(d, p) methods. The computed vibrational frequencies are used to determine the types of molecular motions associated with each of the observed experimental bands. To determine conformational flexibility, molecular energy profile of (1) was obtained by semi-empirical (AM1) calculation with respect to a selected degree of torsional freedom, which was varied from $-180^{\circ}$ to $+180^{\circ}$ in steps of $10^{\circ}$. Molecular electrostatic potential of the compound was also performed by the theoretical method.

• 한국응용약물학회:학술대회논문집
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• 한국응용약물학회 1998년도 Proceedings of UNESCO-internetwork Cooperative Regional Seminar and Workshop on Bioassay Guided Isolation of Bioactive Substances from Natural Products and Microbial Products
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• pp.179-179
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• 1998

We previously reported the hepato-protective effect of butanol soluble fraction of methanolic extract of Carthamus tinctorius L. Semen on carbon tetrachloride induced hepatotoxicity. In this study, the active component from the butanol soluble fraction was isolated by column chromatographic separation using Silica gel and Sephadex LH -20 and identified by spectroscopic methods such as Mass, $^1$H - NMR and $\^$13/C-NMR. The hepato-protective effect of the isolated active component on the CCl$_4$-induced liver damaged rats has been evaluated by performing blood chemical analysis and biotransformational enzyme analysis.

• 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.

• Bulletin of the Korean Chemical Society
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• 제28권6호
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• pp.990-994
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• 2007

Bioassay-guided fractionation of the MeOH extract from the sponge Discodermia calyx collected off the coast of Jeju Island, South Korea, led to the isolation of a polyketide, icadamide C (1), along with previously reported theopederin K (3). Structure elucidation was performed by a combination of high resolution mass and 2D-NMR (principally COSY, HMBC, HSQC, and NOESY) spectroscopy. Stereochemistry of compound 1 was determined as 2R*, 3R*, 6R*, 10S*, 11S*, 12R*, 13S*, 15R* and 2'S by NMR data and Marfey analysis. Isolated metabolites displayed potent cytotoxic activity against a small panel of five human solid tumor cell lines with ED50 values of less than 0.1 μg/mL.

• 대한화학회지
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• 제54권1호
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• pp.49-54
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• 2010

무수탄산칼륨 존재 하에서 2-chloro-N-(4,6-diarylpyrimidin-2-yl)acetamides 25-33를 모르포린과 축합 반응시켜서 2-morpholino-N-(4,6-diarylpyrimidin-2yl)acetamides 34-42 화합물들을 합성하였다. 합성된 화합물들의 녹는점, 원소분석, MS, FT-IR, $^1H$- & $^{13}C$-NMR로 화학적인 구조를 규명되었다.

• 한국식품영양학회지
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• 제24권4호
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• pp.617-621
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• 2011

황련은 염증, 항균, 고혈압 및 항암 작용을 지닌 중요한 전통 한약재이다. 황련 뿌리 메탄올 추출성분은 CPC와 HPLC 방법으로 정제하였다. CPC의 최적 용매 조건은 n-butanol:acetic acid:water(4:1:5)이었다. Berberine(16.8 mg)은 CPC와 HPLC 방법에 의하여 효과적으로 분리하였다. 이 물질의 화학적 구조는 $^1H$, $^{13}C$-NMR과 ESI-MS 데이터 분석에 의하여 확인되었다.