• Title/Summary/Keyword: Solution NMR

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Metal-Dinitrosyl Complexes(III) : Synthesis and Structural Study of Homo-, Hetero-dinuclear Molybdenum and Tungsten Complexes, $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(phen)Cl][ClO_4]_2 $(phen = 1,10-phenanthroline, pyz = pyrazine) (금속-디니트로실 착물 (제 3 보) : 몰리브덴과 텅스텐의 호모 및 헤테로 이핵 착물, $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(phen)Cl][ClO_4]_2 (phen=1,10-phenanthroline,\;pyz=pyrazine)$의 합성 및 구조에 대한 연구)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • v.37 no.7
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    • pp.655-661
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    • 1993
  • The neutral monomeric compounds $[Mo(NO)_2Cl_2(phen)]$ and $[W(NO)_2Cl_2(phen)]$ (phen= 1,10-phenanthroline) have been prepared by reactions of polymeric compounds $[{Mo(NO)_2Cl_2}n],\;[{W(NO)_2Cl_2}n]$ with chelate ligands. Additions of one equivalent of silver(I) perchlorate to these cis-dinitrosyl compounds in acetone solution produce $[Mo(NO)_2(phen)(S)Cl][ClO_4]\;and\;[W(NO)_2(phen)(S)Cl][ClO_4]$ (S = acetone). The homo- and hetero-dinuclear complexes, $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][ClO_4]_2$ (M = Mo, W) and $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][C1O_4]_2$ (M = Mo, M' = W) have been prepared by these monocationic complexes with pyrazine ligand respectively. These complexes characterized by elemental analysis, $1^H-\;and\;^{13}C-NMR$, infrared, and UV-visible spectroscopy are reported. The spectral data indicate that homo- and hetero-dinuclear complexes were symmetrical structures of $C_{2v}$.

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Synthesis and Characterization of Collagen Peptide Based Copolymer from Shaving Scrap (셰이빙 스크랩으로부터 콜라겐 펩타이드계 공중합체 합성과 특성)

  • Park, Min Seok;Shin, Soo Beom;Kim, Ho Soo;Kim, Min Soo;Kim, Ha Sun;Jang, Jae Hyeok;Lee, Jin Kye;Lee, Dong Kuk
    • Applied Chemistry for Engineering
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    • v.33 no.6
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    • pp.581-587
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    • 2022
  • The leather industry generates a large amount of hazardous leather waste of various types every year. Among them, shaving scrap is difficult to recycle because it contains chromium ions. Many studies in recent years have shown that shaving scraps can be processed into various types of valuable products, such as adsorbent, filler, and poultry feed. In this study, collagen peptides were extracted from shaving scraps and structurally modified to be developed as new materials with improved physicochemical properties. First, the chromium ions contained in the shaving scraps were removed using a sodium hydroxide solution, and purified through concentration and low-temperature crystallization. The purified collagen peptide was used to prepare the powder using a spray dryer. The extracted collagen peptides were structurally modified by introducing double bonds by reacting with methacrylic anhydride (MAA), and the product was confirmed by 1H NMR spectroscopy. Next, a copolymer was prepared by redox polymerization of the modified collagen peptide (MCP) and 2-ethylhexyl acrylate (2-EHA). The structure of the copolymer was qualitatively confirmed by FT-IR. In conclusion, this study confirmed that collagen peptides can be extracted from shaving scrap and converted into new eco-friendly materials through certain treatments.

Defence Mechanism of Java Tilapia, Tilapia mossambica, to Clonorchis sinensis (Tilapia mossambica의 간흡충에 대한 방어기전)

  • RHEE Jae-Ku;PAIK Young-Ki;LEE Ho-Il;YANG Hong-Hyun
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.20 no.4
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    • pp.317-327
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    • 1987
  • As a series of studies on the suitability as a second intermediate host of Clonorchis sinensis, artificial infection experiments were applied to Tilapia mossambica. And then, in order to elucidate the defence mechanism of the fish to Clonorchis, clonorchicidal substance in the epidermal mucus of the fish was isolated by silica gel column and thin layer chromatography and analyzed for its chemical structure by UV, IR and NMR-spectroscopy. The results obtained are summarized as follows: 1. The cercariae which attempted to contact with the fish in the water were observed under stereomicroscope. After contact, the cercariae began to separate their tail from the body after several minutes and then the number increased to $80\%$ more than 10 minutes after the encounter. But very few cercariae could actually invade the epidermis of the fish. 2. The fish were reared with Parafossarulus manchouricus which were shedding numerous cercariae of Clonorchis in the aquarium for 24 hours. Only a few cercariae could invade the epidermis but most of the invaded cercariae died out before forming their cysts. Very few number of the remaining encysted cercariae were also found to be in a state of suspended animation within 42 hours. 3. In the cases of the control fish, Pseudorasbora parva, numerous cercariae of Clonorchis were found to invade the fish through the epidermis under stereomicroscope. Then many metacercariae of Clonorchis were also found in the fish while they were kept in the aquarium. 4. A sample of the epidermal mucus of Tilapia mossambica was extracted with ethly ether 6 times repeatedly. In silica gel column chromatography, using petroleum ether: chloroform/30:70(v/v) as a first solvent and MeOH as a second solvent, the extract was fractionated into the yellow and brownish red solutions in the first solvent and the clonorchicidal brownish yellow solution in the second sovent. 5. The clonorchicidal brownish yellow solution was added to petroleum ether, and the mixture was stored for 5 days at $5^{\circ}C$ and was, then, separated into supernatant fraction and precipitate. Ten mg/ml of the supernatant fraction killed, in vitro, the excysted metacercariae in 45 minutes but the precipitate in 600 minutes. 6. In silica gel column chromatography, using acetone: benzene/10:90(v/v) as a solvent, the more clonorchicidal supernatant fraction was fractionated into the first fraction with Rf. 0.2966 and the second fraction with Rf. 0.072. In vitro, 10mg/ml of the first fraction killed the excysted metacercariae in 28 minutes, the second fraction in 80 minutes and the first fraction was, therefore, determined to be a final clonorchicidal substance. 7. By this purification procedures, the most clonorchicidal substance from the epidermal mucus of Tilapia mossambica was purified 71-folds with $0.2075\%$ yield. Infra red, nuclear magnetic resonance and ultraviolet spectrometric analysis of the purified substance revealed that the substance is linoleic acid. According to the results of the present studies it seemed that this species can not serve as a proper intermediate host of Clonorchis sinensis, and that defence mechanism to the fluke seems to be correlated with linoleic acid in the epidermal mucus of this species.

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Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

The Magnetic Relaxation Properties of DTPA-bis(4-carboxycyclohexyl) amide Paramagnetic Gd-chelates (DTPA-bis(4-carboxycyclohexyl)amide 상자성 복합체의 자기이완특성에 관한 연구)

  • Kim, In-Sung;Lee, Young-Ju;Lee, Jae-Jun;Kim, Ju-Hyun;Kim, Yoo-Kyung;Sujit, Dutta;Kim, Suk-Kyung;Kim, Tae-Jeong;Kang, Duk-Sik;Chang, Yong-Min
    • Investigative Magnetic Resonance Imaging
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    • v.10 no.1
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    • pp.20-25
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    • 2006
  • Purpose : To evaluate the NMR relaxation properties of newly developed high performance paramagnetic complexes. Materials and methods : 4-aminomethylcyclohexane carboxylic acid (0.63g, 4 mmol) was mixed with the suspension solution of DMF (15mL) and DTPA-bis-anhydride (0.71g, 2 mmol) to synthesize the ligand. The ligand was then mixed with Gd2O3 (0.18g, 0.5 mmol) to synthesize Gd-chelate. For the measurement of magnetic relaxivity of paramagnetic compounds, the compounds were diluted to 1mM and then the relaxation times were measured at 1.5T(64 MHz). Inversion-recovery pulse sequence was employed for T1 relaxation measurement and CPMG(Carr-Purcell-Meiboon-Gill) pulse sequence was employed for T2 relaxation measurement. Using MATLAB(Version 7.1) program, T1 magnetic relaxation map, R1 map, T2 magnetic relaxation map and R2 map were developed to represent magnetic relaxation time and magnetic relaxivity as image. Results : Compared to $R1=4.9mM^{-1}sec^{-1}$ and $R2=4.8mM^{-1}sec^{-1}$ of Omniscan (Gadodiamide), which is commercially available paramagnetic MR agent, R1 of SUK090(Gd-C32H74N5O24) was $12.46mM^{-1}sec^{-1}$ and R1 of SUK091(Gd-C34H78N5O24) was $12.77mM^{-1}sec^{-1}$. However, R1 of SUK092(Gd-C30H56N5O17) was decreased to $2.09mM^{-1}sec^{-1}$. In case of R2, SUK090(Gd-C32H74N5O24) was $8.76mM^{-1}sec^{-1}$ and SUK091(Gd-C34H78N5O24) was $7.60mM^{-}1sec^{-1}$ whereas SUK092(Gd-C30H56N5O17) was decreased to $1.82mM^{-1}sec^{-1}$. Conclusion : Among three new paramagnetic complexes, SUK090(Gd-C32H74N5O24) and SUK091(Gd-C34H78N5O24) showed higher T1, T2 magnetic relaxation rates than that of commercially available paramagnetic MR agent and thus expected to have more contrast enhancement effect.

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