• 제목/요약/키워드: C-O bond

검색결과 555건 처리시간 0.03초

Synthesis and Reaction Chemistry of Some Ferrocene-Containing Chelate Ligands with Dirhodium Acetate: X-ray Crystal Structure of $(\eta^1-(S,R)-CPFA)_2Rh_2(OAc)_4$

  • Kim, Eun-Jin;Kim, Tae-Jeong
    • Bulletin of the Korean Chemical Society
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    • 제15권11호
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    • pp.990-996
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    • 1994
  • New ferrocene-based chelate amines, $Fe[C_5H_4CH(Me)NMe_2]_2\;(3), \;Fe[C_5H-3(CH(Me)NMe_2)(PPh_2)-1,2]_2\;(4),\;(C_5H_5)Fe(C_5H_3(CH_2NMe_2)(CH(CN)NMe_2-1,2)\;(6),\;and\;(C_5H_5)Fe(C_5H_3(CH_2NMe_2)(CH(Me)NMe_2-1,2)$ (7) have been prepared. The reaction and the coordination chemistry of 4 and other related compounds (S,R)-(1-N,N-dimethylaminoethyl)-2-dicyclohexylphosphino)ferrocene (CPFA) and 1,1'-bis-(diphenylphosphino)ferrocene (BPPF) with $Rh_2(OAc)_4(MeOH)_2$ were investigated. The reaction of the chiral ligand (S,R)-CPFA forms a complex of the type (${\eta}^1$-(S,R)-CPFA-P)$_2Rh_2(OAc)_4$ (8) in which the ligand is coordinated to both rhodium centers in a monodentate fashion through phosphorus. In contrast, the bisphosphine analogues such as BPPF and 4 afford chelate complexes of the type (${\eta}^2-PP)Rh_2(OAc)_4$ (9 & 10) where both ligands act as a chelate bidentate to a single rhodium atom. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of 8 was determined by X-ray crystallography. Crystals are monoclinic, space group C2 (No. 5), with a=26.389 (3), b=12.942 (1), c=11.825 (1) A, ${\beta}$=111.22(1)$^{\circ}$, V=3964.7 (8) $A^3$, Z=4, and $D_{calc}$=1.58 g $cm^{-3}$. Two Rh(II) centers are bridged by four $AcO^-$ groups in the ${\eta}^1$ : ${\eta}^1$ mode across a Rh-Rh single bond, and octahedral coordination at Rh(1) and Rh(1') is completed by axially coordinating (S,R)-CPFA and a briding $AcO^-$, respectively.

플라즈마 용사법에 의한 열차폐 코팅의 열피로에 따른 AE신호 특성 연구 (A Study on Acoustic Emission Characteristics through the Cyclic Thermal Test of Thermal Barrier Coating by Plasma Spray Process)

  • 박진효;이구현;예경환;김승태;전채홍;김정석
    • 한국정밀공학회:학술대회논문집
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    • 한국정밀공학회 2005년도 춘계학술대회 논문집
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    • pp.1349-1352
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    • 2005
  • This paper is to investigate a defect for thermal barrier coating layers by acoustic emission method in 4-point bending test. The two-layer thermal barrier coating is composed of $150\mu{m}\;CoNiCrAlY\;bond\;coating\;by\;vacuum\;plasma\;spray(VPS)\;process\;and\;250\mu{m}\;ZrO_2-8wt%Y_2O_3$ ceramic coating layer by air plasma spray(APS) process on Inconel-718. The specimen prepared by cyclic thermal test(500, 1000, 2000cycle) at $1050^{\circ}C$ The AE monitoring system is composed of PICO type sensor, a wide band pre-amplifier(40dB), PC and AE DSP(16/32 PAC) board. The AE event, amplitude, Cumulative energy and count of coating specimens is evaluated according to cyclic thermal test.

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합성 항산화제가 단백질 분해효소에 미치는 영향-Pepsin의 활성에 미치는 합성 항산화제의 영향 및 기질 Octapeptide의 합성- (The Effect of Synthetic Antioxidants on the proteolytic Enzymes-The Effect of Synthetic Antioxidants on the Activity of the Pepsin and Synthesis of Octapeptide as a Substrate-)

  • 김상옥
    • Journal of Nutrition and Health
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    • 제14권3호
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    • pp.124-128
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    • 1981
  • This study was carried out to understand the activity of pepsin, the proteolytic enzyme, to octapeptide (angiotensin II) in the presence of various synthetic antioxidants as food additives. 1) Dibutyl hydroxy toluene, butyl hydroxyanisole and ethyl protocathechuate did not influence the inhibitory activity of pepsin an the octapeptide as a substrate, but sodium-L-ascorbate inhibited pepsin activity at above 100ppm. However sodium L-ascorbate was completely removed after 30 minutes. 2) Pepsin brought about a quick break up the octapeptide, Asp-Arg-Val-Tyr-Ile-His-Gly-Phe, by splitting the Gly-Phe and Val-Tyr bond. 3) The melting point of synthetized octapeptide was $209-212^{\circ}C$, chemical formula and molecula weight were $C_{43}H_{65}N_{13}O_{12}{\cdot}CH_3COOH{\cdot}H_2O$ and 956.05, respectively. 4) The amino acid mole ratio of synthetized octapeptide by acid hydrolysis were Asp:0.98, Arg: 1.02, Val: 1.00. Tyr: 0.95, Ile: 1.00, His: 1.03, Gly: 0.96, Phe: 1.00.

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Spectroscopic Studies on the High-$T_c$ Superconducting $La_2CuO_{4-δ}$ Prepared by Electrochemical Oxidation

  • 박정철;Alain Wattiaux;Jean-Claude Grenier;김동훈;최진호
    • Bulletin of the Korean Chemical Society
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    • 제18권9호
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    • pp.916-922
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    • 1997
  • A superconducting phase La2CuO4+δ (Tc=44 K) has been prepared by electrochemical oxidation which allows the oxygen to intercalat into the La2O2 layers. According to the Cu K-edge X-ray absorption near edge structure spectroscopic analysis, the oxidized phase shows an overall spectra shift of about 0.5 eV to a higher energy region compared to the as sintered one with the occurrence of an additional peak corresponding to the transition to the |1s13dn+1L-14pσ1 > final state, indicating the oxidation of CuO2 layer. From the X-ray photoelectron spectroscopic studies, it is found that the binding energy of La 3d5/2 is significantly shifted from 834.3 eV (as sintered La2CuO4) to 833.6 eV (as electrochemically oxidized La2CuO4+δ), implying that the covalency of the (La-O) bond is decreased due to the oxygen intercalation. The O 1s spectra do not provide an evidence of the superoxide or peroxide, but the oxide (O2-) with the contaminated carbonate (CO32-) based on the peaks at 529 eV and 532 eV, respectively, which is clearly confirmed by the Auger spectroscopic analysis. Oxygen contents determined by iodometric titration (δ=0.07) and thermogravimetry (δ=0.09) show good coincidence each other, also giving an evidence for the "O2-" nature of excess oxygen. From the above results, it is concluded that "O2-" appeared as O 1s peak at 528.6 eV is responsible for superconductivity of La2CuO4+δ.

1,3-Diazatricyclo[5.3.1.$0^{5,11}$ undecane-2,4-dione의 합성과 결정구조 (Synthesis and Crystal Structure of 1,3-Diazatricyclo[5.3.1.$0^{5,11}$] undecane-2,4-dione)

  • 김정욱;윤호섭
    • 한국결정학회지
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    • 제5권2호
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    • pp.100-107
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    • 1994
  • 분자내 (2+2) 광고리화 반응을 통하여 pyridine의 새로운 N1-pentenyl유도체가 얻어졌다. 이 물질의 구조는 단 결정 X-선 회절법에 의해 해석되었다. 이 화합물은 rhombohedral계( R3, a=27.767(5)A, c=6.390(2)A)로 결정화된다. 이 구조에서는 2개의 6각 고리와 1개의 4각 고리가 N-C 또는 C-C bonds를 공유하면서 fuse되어 있고, pyridine고리는 의자모양의 형태를 취하고 있다. 점대칭으로 연관된 한 쌍의 분자들이 uracil 부분의 N,0 원자 사이의 H를 통하여 수소결합을 생성하고 있는 것이 관찰되었다.

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질화규소에 의한 SiC 소결체의 제조에 관한 연구 (Febrication of $Si_3-N_4$ Bonded SiC Ceramics)

  • 정주희;김종희
    • 한국세라믹학회지
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    • 제20권1호
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    • pp.63-69
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    • 1983
  • It is know that $Si_3-N_4$ bonded SiC has almost all the valuable properties needed for the high temperature material and thus has bery wide range of applicability. Si powder and two different sized SiC powder were used as the raw mateials. Specimens were prepared by heating the green compact mode of the raw materials with polyvinyl alcohol binder in the nitrogen atmosphere. The bond-ing of SiC particles is brought about with the formation of reaction bonded silicon nitride phase between the particles he influences of the variation of the relative amounts of the raw materials and the amount of the organic binder on the density and the bend strength of the specimens were investigated. It was shown that the calculation of the amount of the nitridation of Si is somewhat complicated matter since some portion of the organic binder reacts with the Si during the firing process. Fixing the Si amount to 20w/o the distributions of the size of the SiC particles that gives the maximum density and the maximum strnegth were obtained through experiments. It was observed that the two distributions were not equal to each other. As the amount of Si increased the amount of Si reacted with nitrogen and the strength increased. The fracture mode was intergranular for the most part and the transgranular fracture was scarcely observed.

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Recent advances in carbon-11 chemistry

  • Lu, Yingqing;Lee, Byung Chul;Kim, Sang Eun
    • 대한방사성의약품학회지
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    • 제2권1호
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    • pp.9-16
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    • 2016
  • Carbon-11 is one of the most sensitive and desirable positron emission tomography radio-isotope, which offers the capacity to be incorporated, through a covalent bond, into biologically active molecules without altering their biological properties. Carbon-11 can be obtained from the cyclotron with two different chemical forms: $[^{11}C]CO_2$ and $[^{11}C]CH_4$. [$^{11}C$]Methyl iodide has been widely used as a highly reactive labelling precursor that can be applied to label carbon-11 with biologically active molecules via alkylation of N-, O-, or S-nucleophiles. A more recent and still challenging labeling method is transition metal mediated $^{11}C$-carbonylation. Advances in organic chemistry, radiochemistry and improved automated techniques greatly encourage researchers to develop more carbon-11 labelled radiotracers for molecular imaging studies. This mini-review will introduce a historical track of carbon-11 chemistry combining with examples and its role in near future.

Comparative Evaluation of Mn(II) Framework Substitution in MnAPSO-34 and Mn-impregnated SAPO-34 Molecular Sieves Studied by Electron Spin Resonance and Electron Spin Echo Modulation Spectroscopy

  • Gernho Back;Kim, Yanghee;Cho, Young-Soo;Lee, Yong-Ill;Lee, Chul-Wee
    • 한국자기공명학회논문지
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    • 제6권1호
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    • pp.20-37
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    • 2002
  • MnAPSO-34 and Mn-impregnated SAPO-34(Mn-SAPO-34) sample were prepared with various manganese contents and studied by electron spin resonance(ESR) and electron spin echo modulation(ESEM). Electron spin echo modulation analysis of 0.07mo1 % Mn(relative to p) in MnAPSO-34 with adsorbed D$_{2}$O shows two deuteriums at 0.26 nm and two at 0.36 nm from Mn. This suggests that two waters hydrate an MnO$_{4}$ configuration with a D-O bond orientation for the waters as expect for a negatively charged site at low manganese content (0.1 mol%), the ESR spectra of MnAPSO-34 and MnH-SAPO-34 exhibit the same parameters(g 2.01 and A 89 G), but the spectra obtained from MnAPSO-34 samples are better resolved. The decomposition temperature of as-synthesized MnAPSO-34 were in the range of 200-600 $^{\circ}C$ of the morpholine which is 12 $^{\circ}C$ higher than that in as-synthesized MnH-SAPO-34. Infrared spectra showed that the position of a band at 3450 $cm^{-1}$ / shifted about 15 $cm^{-1}$ / toward higher energy in MnAPSO-34 versus MnH-SAPO-34. The modulation depth of the two-pulse ESE of MnAPSO-34 with adsorbed D$_{2}$O is deeper than that of MnH-SAPO-34 with adsorbed D$_{2}$O. Three-pulse ESEM of MnAPSO-34 and MnH-SAPO-34 with adsorbed deuterium oxide shows that the local environments of manganese in the hydrated samples are different, suggesting that Mn(II) is framework substituted in MnAPSO-34 since it obviously occupies an extraframework position in MnH-SAPO-34.

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Comparative Evaluation of Mn Substitution in a Framework Site in MnAPSO-34 and Mn-impregnated SAPO-34 Molecular Sieves Studied by Electron Spin Resonance and Electron Spin-Echo Modulation Spectroscopy

  • Gernho Back;Cho, Young-Soo
    • 한국자기공명학회:학술대회논문집
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    • 한국자기공명학회 2002년도 International Symposium on Magnetic Resonance
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    • pp.80-80
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    • 2002
  • MnPSO-34 and Mn-impregnated SAPO-34 (Mn-SAPO-34) sample were prepared with various manganese contents and studied by electron spin resonance (ESR) and electron spin-echo modulation (ESEM). Electron spin-echo modulation analysis of 0.07mol % Mn(relative to p) in MnAPSO-34 with adsorbed D$_2$O shows two deuteriums at 0.25 nm and two at 0.36 nm from Mn. This suggests that two waters hydrate an MnO4 configuration with a D-O bond orientation for the waters as expect for a negatively charged site at low manganese content (0.07 mol%), the ESR spectra of MnAPSO-34 and MnH-SAPO-34 exhibit the same parameters (g 2.02 and A 87 G), but the spectra obtained from MnAPSO-34 samples are better resolved. TGA of as-synthesized MnAPSO-34 shows that the decomposition temperature in the range 200-$600^{\circ}C$ of the morpholine is 12$^{\circ}C$ higher than that in as-synthesized MnH-SAPO-34. Infrared spectra shows that the position of a band at about 15 cm-1 toward higher energy in MnAPSO-34 versus MnH-SAPO-34. The modulation depth of the two-pulse ESE of MnAPSO-34 with absorbed D$_2$O is deeper than that of MnH-SAPO-34 with absorbed D$_2$O. Three-pulse ESEM of MnAPSO-34 and MnH-SAPO-34 with absorbed deuterium oxide shows that the local environments of manganese in the hydrated samples are different, suggesting that Mn(II) is framework substituted in MnAPSO-34 since it obviously occupies an extra-framework position in MnH-SAPO-34

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Electrical, Electronic Structure and Optical Properties of Undoped and Na-doped NiO Thin Films

  • Denny, Yus Rama;Lee, Kangil;Seo, Soonjoo;Oh, Suhk Kun;Kang, Hee Jae;Yang, Dong-Seok
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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    • pp.193.1-193.1
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    • 2014
  • This study was to investigate the electronic structure and optical properties of Na doped into NiO thin film using XPS and REELS. The films were grown by electron beam evaporation with varying the annealing temperature. The relationship between the electrical characteristics with the local structure of NiO thin films was also discussed. The x-ray photoelectron results showed that the Ni 2p spectra for all films consist of Ni 2p3/2 which indicate the presence of Ni-O bond from NiO phase and for the annealed film at temperature above $200^{\circ}C$ shows the coexist Ni oxide and Ni metal phase. The reflection electron energy loss spectroscopy spectra showed that the band gaps of the NiO thin films were slightly decreased with Na-doped into films. The Na-doped NiO showed relatively low resistivity compared to the undoped NiO thin films. In addition, the Na-doped NiO thin films deposited at room temperature showed the best properties, such as a p-type semiconducting with low electrical resistivity of $11.57{\Omega}.cm$ and high optical transmittance of ~80% in the visible light region. These results indicate that the Na doping followed by annealing process plays a crucial in enhancing the electrical and optical properties of NiO thin films. We believe that our results can be a good guide for those growing NiO thin films with the purpose of device applications, which require deposited at room temperature.

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