• 대한화학회지
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• 제55권2호
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• pp.317-322
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• 2011

• 대한화학회지
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• 제56권3호
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• pp.357-362
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• 2012

5-Nonylsalicylaldoxime and salicylaldehyde are two derivatives of phenolic compounds which are very applicable materials in industries. Formerly the formylation of phenolic derivatives were carried out by Rimer-Tiemann method. In this work both of these two materials were synthesized by magnesium meditated formylation technique and their structural characterizations were compared by instrumental analysis technique. In order to achieve a selectively orthoformylated product, the hydroxyl group of nonylphenol (or phenol) was first modified by magnesium methoxide. The nonylphenol magnesium salt was then formylated by paraformaldehyde. The oximation reaction was finally applied to the prepared nonylsalicylaldehyde magnesium salt by liquid extracting via water and acid washing and other extractions. The solvent was finally removed by evaporation under reduced pressure. Some instrumental analysis such as $^1H$-NMR, GC/MS and FT-IR spectra were taken on the product in order to interpret the reaction characterization quantitatively and qualitatively. The formaldehyde and oxime functional groups of two compounds were investigated through $^1H$-NMR and FT-IR spectra and were compared. The yield of methoxilation was very good and the yields of formylation and oximation reactions were about 90%and 85% respectively. The orthoselectivity of formylation reaction were evaluated by comparing of the relevant spectra. The GC/MS spectra also confirmed the obtained results.

• Archives of Pharmacal Research
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• 제22권2호
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• pp.143-150
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• 1999

melatonin (MLT), N-acetyl-5-methoxytryptamine, is mainly secreted by the pineal gland. The ultraviolet (UV), infrared (IR) and 1H-NMR spectra of irradiated and non-irradiated MLT were measured, and phototoxicity tests of MLT, anthracence (positive control) and sodium lauryl sulfate (SLS, negative control) were performed. The methods employed include both in vitro test such as MTS assay using the human fibroblast cell and yeast growth inhibition assay using Candida albicans and in vivo method using the skin of guinea pig. UV absorption spectra and 1H-NMR spectra of MLT were changed by UVA (365 nm, 15 J/$\textrm{cm}^2$), but IR spectra of MLT were not changed. The fifty percent inhibitory concentration (IC50) ratio (UV-/UV+) of MLT was 10. The inhibition zone of irradiated-paper disks treated with MLT was not observed. According to the results of histophathological examination, no pathologic lesion was observed in the non-irradiated group, but slight degeneration of keratinocytes in the epidermis, homorrhage and vasodilation in dermis were observed in the irradiated group. These results indicated that the molecular structure of MLT is altered by UVA to unidentified photoproducts and a moderate phototoxicity of MLT is predicted.

• Bulletin of the Korean Chemical Society
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• 제32권1호
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• pp.229-238
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• 2011

A series of novel glucose derived benzyl and alkyl 1,2,3-triazoles and their hydrochlorides have been synthesized via Cu(I)-catalyzed 1,3-dipolar cycloaddition. All the new compounds were characterized by MS, IR and NMR spectra. The DEPT, APT, $^1H$-$^1H$ and $^1H-^{13}C$ 2D NMR spectra for some compounds were also recorded. These compounds were evaluated for their in vitro antibacterial activities against Staphylococcus aureus ATCC 29213, Bacillus subtilis, Bacillus proteus, Pseudomonas aeruginosa, Escherichia coli ATCC 25922, and antifungal activities against Candida albicans and Aspergillus fumigatus. The bioactive data revealed that (3R,4S,5S,6S)-2-(hydroxymethyl)-6-methoxy-4,5-bis((1-octyl-1H-1,2,3-triazol-4-yl)methoxy)-tetrahydro-2H-pyran-3-ol 8a exhibited excellent antifungal activity against A. fumigatus with an MIC value of 0.055 mM compared to Fluconazole. It also showed broad inhibitory efficacy against tested bacterial strains with MIC values ranging from 0.049 mM to 0.39 mM.

• 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.

• 한국자기공명학회논문지
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• 제15권1호
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• pp.14-24
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• 2011

We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.

• Bulletin of the Korean Chemical Society
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• 제18권9호
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• pp.961-965
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• 1997

1H NMR spectra of 3,3-dimethylpiperidine (1) at -70 to 30 ℃ exhibit gradual change from slow to rapid exchange between two alternate chair forms. The exchange rate constant was determined as a function of temperature by simulating the line shape of the signal from the two methyl groups using the modified Bloch equations. The resulting free energy of activation is ΔG* = 44.4±1.9 kJ mol-1 at 298 K. The 1H NMR spectrum of a D2O or dimethylsulfoxide-d6 (DMSO-d6) solution containing 1 and [SiW11CoⅡO39]6- exhibits separate signals for the free ligand and the complex, indicating that the ligand exchange is slow on the NMR time scale. In D2O the piperidine ring is frozen as a chair form even at room temperature with the cobalt ion bonded to the axial position of the nitrogen atom. When DMSO-d6 is added to the D2O solution, the NMR spectral change suggests that a rapid exchange occurs between the chair form and another conformer. It is proposed that the conformation of ^b1^b coordinated to [SiW11CoⅡO39]6- in DMSO-d6 is close to a twist form.

• 광물과 암석
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• 제34권1호
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• pp.31-40
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• 2021

명목상의 무수 광물의 수소 원자는 격자의 결함에 존재하는 것으로 알려져 있지만, 나노 스케일 입자의 경우 입자 표면에 물과 수산기의 형태로 존재할 수 있다. 본 연구에서는 비정질 규산염 나노입자의 수소 원자 환경에 대한 정량 측정 방법으로서, 1H 고상 핵자기 공명(solid-state nuclear magnetic resonance, NMR) 분광분석의 실효성을 알아보고자 하였다. 온도와 습도가 조절되는 글러브 박스 내에서 NMR 로터에 패킹된 비정질 규산염 나노입자를 25%와 70 % 상대습도에서 2일에서 10일까지 동안 보관한 후 1H NMR 스펙트럼을 측정한 결과, 약간의 차이는 있었으나 큰 변화가 관찰되지 않았다. 이는 NMR 로터에 패킹된 시료의 수소 원자 환경이 외부 대기에 의해 거의 변화하지 않았음을 의미한다. 수화 시간에 따른 비정질 규산염 나노입자의 함수량은 약 10 % 범위에서 차이를 보이며, 이는 글러브 박스의 시간적, 공간적 습도 불균일성에 의한 것으로 생각된다. 1H NMR 스펙트럼의 정량 분석 결과, 수화 상대습도가 증가함에 따라 비정질 규산염 나노입자의 수소 원자 수 역시 선형적으로 증가하였다. 이와 같은 결과는 NMR 로터의 시료 밀폐 능력이 수화 환경을 보존하며, 대기 상대습도 변화에 따른 나노입자의 함수량 변화 측정에 적합함을 의미한다. 본 연구의 결과를 통해, 1H 고상 핵자기 공명 분광분석을 이용하여 나노 스케일의 명목상의 무수 광물의 표면적, 결정도가 습도에 따른 광물의 함수량 변화에 미치는 영향에 대한 체계적인 연구를 할 수 있을 것으로 기대된다.

• Bulletin of the Korean Chemical Society
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• 제7권6호
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• pp.433-438
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• 1986

Two new types of NMR shift reagents, one giving dipolar-only and the other giving contact-only shifts, can be prepared simply by mixing two appropriate $Ln(fod)_3$(Ln = Pr, Nd, Eu, and Yb) reagents in certain ratios. The $^1H$ and $^{13}C$ NMR spectra of pyridine-type substrates, quinoline and isoquinoline, whose paramagnetic shifts are normally a composite of contact and dipolar contributions with single lanthanide shift reagents, show the feasibility of this approach.

• Journal of the Korean Wood Science and Technology
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• 제41권6호
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• pp.566-575
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• 2013

주목열매에서 분리한 과육과 씨를 95% EtOH 용액을 사용하여 각각 1.15 kg과 0.94 kg을 유리 용기에 침지하여 추출하고, 농축된 추출용액을 용매의 극성에 따라 n-hexane, dichloromethane, ethyl acetate 및 수용성으로 순차 분획한 후, 동결건조하였다. 혼합물로부터 순수한 화합물을 분리하기 위하여 ethyl acetate 및 수용성 분획에 대하여 Sephadex-LH 20 칼럼크로마토그래피를 실시하였다. 단리된 화합물들의 구조는 flavan 화합물의 경우 $^1H$-NMR, $^{13}C$-NMR 및 EI-MS 스펙트럼을 측정하였으며, 탄수화물은 보다 정확한 구조를 결정하기 위해 COSY, HSQC와 같은 2-D NMR과 LC/MS 스펙트럼을 이용하여 구조를 결정하였다. 또한 구성당 분석을 위해 acid hydrolysis, permethylation을 실시하여 구성당의 성분과 결합위치를 확인하였다. 위의 실험을 통하여 (+)-catechin (1), (-)-epicatechin (2), (+)-gallocatechin (3), (-)-epigallocatechin(4) 및 ${\beta}$-D-fructofuranose-($2{\rightarrow}4$)-O-${\beta}$-D-glucopyranose($1{\rightarrow}4$)-O-${\alpha}$-D-glucopyranose-($1{\rightarrow}2$)-O-${\beta}$-D-fructofuranose (5)의 구조를 결정하였다.