• 제목/요약/키워드: 31P NMR

검색결과 123건 처리시간 0.018초

포스핀류가 배위된 팔라듐 착물에 의한 불포화카르복실산의 카르보닐화고리 반응 (제 1 보). 불포화카르복실산이 배위된 팔라듐(0, Ⅱ) 착물의 합성과 구조 (Carbonylative Cyclization of Unsaturated Carboxylic Acids by Palladium Complexes with Phosphines(I) Synthesis and Structure of Palladium(O, II) Complexes with Unsaturated Carboxylic Acids)

  • 도명기;정맹준;이동진
    • 대한화학회지
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    • 제37권4호
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    • pp.423-430
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    • 1993
  • $trans-PdEt_2(PMe_3)_2$와 styrene을 반응시켜 얻어진 $Pd(PMe_3)_2$(styrene)에 methacrylic acid와 trans-crotonic acid를 각각 반응시켜 새로운 팔라듐(O)-올레핀착물로서 $(PMe_3)_2Pd{CH_2=C(CH_3)COOH}$(PMe_3)_2Pd{(CH_3)CH=CHCOOH}$를 합성하고, 구조와 특성을 원소분석, IR 및 $^1H-,\;^{13}C-,\;^{31}P-NMR$ 등의 분광학적 방법으로 조사하였다. methacrylic acid 와 trans-crotonic acid에 존재하는 올레핀의 이중결합은 팔라듐(O)에 ${\pi}$-결합을 형성하였고, 카르복실산은 팔라듐에 결합되지 않았음을 알게되었다. 그리고 동일한 반응에서 metallacycle을 형성하는 3-butenoic acid와 비교 검토하였다.

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Synthesis and Structure of $[Ni(dppe)_2] (dppe=Ph_2PCH_2CH_2PPh_2)$ ($[Ni(dppe)_2]$의 합성 및 구조)

  • Kim, Wan -Sung;Lee, Ji-Hwa;Lee, Soon W.
    • 한국결정학회지
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    • 제11권2호
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    • pp.80-83
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    • 2000
  • Compound [Ni(P(OEt)3)4] (1) reacted with bis(diphenylphosphino)ethane (Ph2PCH2CH2Ph2, dppe) to give bis(bis(diphenylphosphine)ethane)nickel(0), [Ni(dppe)2] (2). Compound 2 was characterized by spectroscopy (1H-and 31P{1H}-NMR) and X-ray crystallography. Crystallographic data for 2: monoclinic space group P21/n, a=9.826(1)Å, b=21.167(2)Å, c=21.425(2)Å, β=91.957(9)°, Z=4, R(wR2)=0.0377(0.0882).

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Synthesis of Novel Halobenzyloxy and Alkoxy 1,2,4-Triazoles and Evaluation for Their Antifungal and Antibacterial Activities

  • Wan, Kun;Zhou, Cheng-He
    • Bulletin of the Korean Chemical Society
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    • 제31권7호
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    • pp.2003-2010
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    • 2010
  • A new class of halobenzyloxy or alkoxy 1,2,4-triazoles and their hydrochlorides were synthesized through cyclization starting from commercially available phenylhydrazine. The structures were characterized by MS, IR and $^1H$ NMR spectra as well as elemental analyses. All the synthesized compounds were screened for their antibacterial activities in vitro against Staphylococcus aureus (ATCC29213), methicillin-resistant Staphylococcus aureus (N315), Bacillus subtilis, Escherichia coli (ATCC25922), Pseudomonas aeruginosa, Shigella dysenteriae, Eberthella typhosa, and antifungal activities against Candida albicans (ATCC76615), Aspergillus fumigatus by broth microdilution assay method. The results of preliminary bioassay indicated that 3-(2,4-difluorobenzyloxy)-1-phenyl-1H-1,2,4-triazole hydrochloride exhibited the best inhibitory activity with an MIC value of 56.25 ${\mu}M$ against P. aeruginosa superior to Chloramphenicol, and showed comparable activity with Chloramphenicol against E. coli (ATCC25922).

Synthesis and Antibacterial Evaluation of Some Novel 2-Arylamino-4-phenyl-thiazolyl Derivatives

  • Parmar, Kokila A.;Suthar, Bharat G.;Parajapati, Sarju
    • Bulletin of the Korean Chemical Society
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    • 제31권4호
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    • pp.793-797
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    • 2010
  • A series of 2-aminothiazoles derivatives have been synthesized and tested for in vitro antibacterial activity on different microorganisms. Syntheses have been carried out following simple methodology in excellent isolated yields. The structure and purity of the original compounds were confirmed by IR, NMR, Mass spectroscopy, and elemental analysis. All compounds were tested for antibacterial activity against S. aureus, S. pyogenes, E. coli, P. aeruginosa, S. typhi and V. parahaemolyticus. These preliminary results indicate that some of compounds are exhibiting good activity.

Synthesis and Reactivity of the Pentacoordinate Organosilicon and -germanium Compounds Containing the C,P-Chelating ο-Carboranylphosphino Ligand [ο-C2B10H10PPh2-C,P](CabC,P

  • Lee, Tae-Gweon;Kim, Sang-Hoon;Kong, Myong-Seon;Kang, Sang-Ook;Ko, Jae-Jung
    • Bulletin of the Korean Chemical Society
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    • 제23권6호
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    • pp.845-851
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    • 2002
  • The synthesis of the intramolecular donor - stabilized silyl and germyl complexes of the type ($Cab^c.p) MMe_2X$ (2a:M=Si, X=Cl;2b;M= Ge, X=Cl;2e;M=Si,X=H) was achieved by the reaction of $LiCab^c,p$ (1) with $Me_2SiClX$ and $Me_2GeCl_2$ respectively. The intramolecular M←P interacion in 2a-2c is provided by $^1H$, $13^C.$, $31^P$ and $29^Si$ NMR spectroscopy. The salt elimination reactions of dichlorotetramethyldisilane and -digermane with 1 afforded the $bis(\sigma-carboranylphosphino)disilane$ and disgermane [$(Cab^C.P)MMe_2]_2(4a;M$ = Si;4b: M=Ge). The oxidative addition reaction of 4a-4b with $pd_2(dba)_3CHCl_3afforded$ the bis(silyl)-and bis(germyl)-palladium complexes. The chloro-bridged dipalladium complexes were obtained by the reaction of 2a-2b with $pd_2(dba)_3CHCl_3$ The crystal structures of 5a and 7b were determined by X-ray structural studies.

2-DDG가 FSa II 종양의 성장속도와 증식 능력, 신진대사에 미치는 영향 ; $^{31}P$-자기공명 분광기와 유세포 분석기를 이용한 연구 (Effects of 2-Deoxy-D-Glucose on Metabolic Status, Proliferative Capacity and Growth Rate of FSall Tumor: Observations made by In Vivo $^{31}P$-Nuclear Magnetic Resonance Spectroscopy and Flow Cytometry)

  • 장혜숙;최은경;조정길;임태환;이대근;이윤;조영주;김곤섭
    • Radiation Oncology Journal
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    • 제9권1호
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    • pp.1-6
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    • 1991
  • 2-ODG가 쥐의 섬유육종(FSall)에 미치는 영향에 대한 연구로 에너지 신진대사는 체내에서의 $^{31}P$-자기공명 분광기를 이용하여 관찰하였고 세포 증식 능력은 유세포 분석기를 사용하여 연구하였다. 성장속도는 10개의 세포를 $C_3Hf/Sed$ 쥐의 발등에 이식한 후 3차원적으로 측정하여 관찰하였다. 2-DDG를 투여한 경우에는 이식후 12일에 복강내로 주사하였다. 이식후 12일의 종양의 평균 크기는 $250mm^3$이었다. Fsall종양의 성장속도는 semilog graph의 기울기와 종양의 doubling time으로 측정하였다. 2-DDG를 투여한 후 성장속도가 감속되었다. 5~12일 사이의 성장속도의 기울기가 0.828, 종양의 Idubling time이 0.84일이고 대조군에서는 13~28일 사이의 기울기가 0.218, doubling time이 3.2일인 반면 2-DOG 투여군에서는 성장속도의 기울기가 0.135이고 doubling time이 5.1일이었다. $^{31}P$-자기공명 분광기를 이용하여 2-DDG의 영향을 분석해 본 결과 2-DDG 투여후 종양증식 속도의 감속과 더불어 phosphornonester (PME)와 inorganic phosphate (Pi)의증가속도가 감소하였다. 이것은 2-DDG투여후 세포의 괴사가 감소하였다는 의미가 있다. 유세포 분석기를 이용하여 종양의 증식 능력을 분석한 결과는 2-DDG 투여후 5-phase와 G2+M phase의 DNA분포가 크게 증가하였다. 이것은 2-DDG투여후 세포가 좀더 방사선에 민감한 cycle로 진행함을 의미하는 것으로 해석할 수 있다. 이에 저자들은 2-DDG가 Fsall 종양세포에 미치는 흥미있는 결과를 토대로 방사선 치료에 미치는 영향과실제 이용 가능성에 대하여 더 연구하고자 한다.

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Preparation and Characterization of Dinuclear Metal Complexes, $[(PPh_3)_2(CO)M({\mu}-E)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (M = Rh, Ir; E = 1,4-Dicyanobenzene and 1,4-Dicyano-2-butene)

  • Moonsik Kim;JaeKyun Chin;Jaejung Ko
    • Bulletin of the Korean Chemical Society
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    • 제13권5호
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    • pp.556-559
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    • 1992
  • Hydrocarbon solution of $(PPh_3)_2(CO)MOSO_2CF_3$ (M= Rh, Ir) reacts rapidly with 1,4-dicyanobenzene or 1,4-dicyano-2-butene to yield dinuclear metal complexes $[(PPh_3)_2(CO)M({\mu}-dicyanobenzene)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (I: M = Rh; II: M = Ir) or $[(PPh_3)_2(CO)M({\mu}-dicyano-2-benzene)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (III: M = Rh; IV: M = Ir), respectively. Compounds I, II, III, and IV were characterized by $^1H$-NMR, $^{31}P$-NMR, and infrared spectrum. Dichloromethane solution of II and IV reacts with $H_2\;and\;I_2$ to yield oxidative addition complexes $[(PPh_3)_2(CO)IrX_2({\mu}-E)X_2Ir(CO)(PPh_3)_2](SO_3CF_3)_2$ (V; E = 1,4-dicyanobenzene, $X_2$ = $H_2$; VI : E = 1,4-dicyano-2-butene, $X_2$ = $H_2$; VII; E = 1,4-dicyanobenzene, $X_2$ = $I_2$). All metal complexes are bridged by the cyanide groups. Compounds Ⅴ, Ⅵ, and Ⅶ are characterized by conventional methods.

The Ir(PPh$_3)_2\;(CO)OClO_3\;and\;Ir(PPh_3)_3N_2Cl$ Mediated Activation of Aldehyde C-H Bonds via Chelate-Assisted Oxidative Addition

  • Ko, Jae-Jung;Joo, Wan-Chul;Kong, Young-Kun
    • Bulletin of the Korean Chemical Society
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    • 제7권5호
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    • pp.338-341
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    • 1986
  • Hydrocarbon solution of $Ir(PPh_3)_2(CO)OClO_3$ reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to yield ${\bar{Ir(Ph_2PC_6H_4-o-CO)}}\;(PPh_3)_2(CO)(H)ClO_4$(1) and ${\bar{Ir(NC_6H_6NC}}C_6H_5)(PPh_3)_2(CO)(H)ClO_4$(2), respectively. The compound $Ir(PPh_3)_2N_2Cl$ also reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to give ${\bar{Ir(Ph_2PC_6H_4-o-C}}O)(PPh_3)_2(H)Cl(3)$ and $Ir(NC_6H_5NCC_6H_5(PPh_3)_2(H)Cl(4)$, respectively. Compounds 1, 2, 3, and 4 were characterized by infrared, $^1H$ NMR, $^{31}p$ NMR, UV spectra, and conductivity measurements.

Engineering and Characterization of the Isolated C-Terminal Domain of 5-Enolpyruvylshikimate-3-phosphate (EPSP) Synthase

  • Kim, Hak-Jun;Kim, Hyun-Woo;Kang, Sung-Ho
    • Journal of Microbiology and Biotechnology
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    • 제17권8호
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    • pp.1385-1389
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    • 2007
  • 5-Enolpyruvylshikimate-3-phosphate (EPSP) synthase catalyzes the formation of EPSP and inorganic phosphate from shikimate-3-phosphate (S3P) and phosphoenolpyruvate (PEP) in the biosynthesis of aromatic amino acids. To delineate the domain-specific function, we successfully isolated the discontinuous C-terminal domain (residues 1-21, linkers, 240-427) of EPSP synthase (427 residues) by site-directed mutagenesis. The engineered C-terminal domains containing no linker (CTD), or with gly-gly ($CTD^{GG}$) and gly-ser-ser-gly ($CTD^{GSSG}$) linkers were purified and characterized as having distinct native-like secondary and tertiary structures. However, isothermal titration calorimetry (ITC), $^{15}N-HSQC$,\;and\;^{31}P-NMR$ revealed that neither its substrate nor inhibitor binds the isolated domain. The isolated domain maintained structural integrity, but did not function as the half of the full-length protein.

Synthesis and Molecular Structure of Tetrahomodioxa p-Phenylcalix[4]arene Tetra Ester Derivative in 1,4-Alternate Conformation

  • 노관현;박영자;최은주
    • Bulletin of the Korean Chemical Society
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    • 제20권8호
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    • pp.905-909
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    • 1999
  • Reaction of tetrahomodioxa p-phenylcalix[4]arene with ethyl bromoacetate and potassium carbonate in ace-tone leads to the title tetra ester derivative, 7,13,21,27-tetra-phenyl-29,30,31,32 -tetrakis(ethoxycarbonyl)meth-oxy-2,3,16,17-tetrahomo-3,17-dioxacalix[4]arene, its structure was determined by NMR spectra as 1,4-alternate conformation. The molecular structure has been solved by X-ray diffraction methods. The molecule has a conformation with pseudo center of symmetry. The benzene ring A is up, ring C is down, B and D rings are flat with respect to the plane of the macrocyclic ring.