• Title/Summary/Keyword: PPh3

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Synthesis of $Cp^*Ru(CO)(PR_3)H$ Type Complexes and Photo-Induced H/D Exchange Reaction ($Cp^*Ru(CO)(PR_3)H$형 착물의 합성과 광반응에 의한 H/D 교환반응)

  • Lee, Dong Hwan;Kim, Sng Il;Kim, Jang Il;Oh, Yung Hee;Kam, Sang Kyu
    • Journal of the Korean Chemical Society
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    • v.41 no.12
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    • pp.645-652
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    • 1997
  • Hydride complexes Cp*Ru(CO)(PR3)H (Cp*=η5-C5Me5, PR3=PMe3, PEt3, PMePh2, PPh3, PCy3)(4a-4f) were synthesized by the reaction of the corresponding chloro complex Cp*Ru(CO)(PR3)Cl (3a-3f) with various hydridic reagent (NaBH4, LiAlH4, LiBEt3H) or NaOMe. Irradiation of Cp*Ru(CO)(PCy3)H (5e) in C6D6 solution with UV light caused H/D exchange reaction between coordinated Cp*, PCy3 and/or Ru-H ligand proton and a deuterium of the deuterated aromatic solvent through a series of inter- and intramolecular C-H activation. The proposed mechanism was described.

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Ruthenium Catalyzed Synthesis of N-Substituted Perhydroazepine Derivatives (루테늄 촉매를 이용한 N-치환 과수소아제핀 유도체의 합성)

  • Sim, Sang Cheol;Do, Chil Hun;Lee, Seung Yeop;Jo, Wan Ho;Heo, Geun Tae
    • Journal of the Korean Chemical Society
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    • v.34 no.6
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    • pp.652-657
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    • 1990
  • Primary amines react with 1,6-hexanediol at 180$^{\circ}C$ for 5 h under argon atmosphere in the presence of both $RuCl_3{\cdot}3H_2$O and $PR_3$ to give N-substituted perhydroazepine derivatives in good yields. For aromatic amines such as anilines, $RuCl_3{\cdot}3H_2$O combined with $PPh_3$ showed the highest catalytic activity. On the other hand, in the reaction of aliphatic amines, $RuCl_3{\cdot}3H_2$O combined with $PBu_3$ showed the highest catalytic activity. These differences may be attributed to the difference in the basicity of these amines. Less basic aromatic amines may require less basic phosphines, while more basic aliphatic amines may require more basic phosphines as the ligands.

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Synthesis of $Cp^*Ru(CO)Cl_2(Cp^*={\eta}^5-C_5Me_5)$ Complex and Reaction with Phosphines ($Cp^*Ru(CO)Cl_2(Cp^*={\eta}^5-C_5Me_5)$착물의 합성과 포스핀과의 반응)

  • Lee, Dong Hwan;Kim, Sng Il;Jun, Jin Hee;Oh, Yung Hee;Kam, Sang Kyu
    • Journal of the Korean Chemical Society
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    • v.41 no.12
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    • pp.639-644
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    • 1997
  • Novel carbonylruthenium (Ⅲ) complex Cp*Ru(CO)Cl2(2, Cp*=η5-C5Me5) was synthesized by the reaction of [Cp*RuCl2]2(1) with CO in toluene. The effective magnetic moment (Veff=1.81 B.M.) derived from the magnetic susceptibility measurement of the complex (2) was consistent with the presence of one "single" unpaired electron. Dibromocarbonylruthenium (Ⅲ) complex Cp*Ru(CO)Br2(3) was obtained by the reaction of complex (2) with KBr in toluene. Complex (2) was easily reduced by the reaction with phosphine in toluene to give the corresponding Ru (Ⅱ) complex Cp*Ru(CO)(PR3)Cl (4a∼4e, PR3=PMe3, PEt3, PMePh2, PPh3, PCy3).

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Palladium-Catalyzed Cross-Coupling Reaction of (E)-1-Alkenyl-1,3,2-benzo-dioxaboroles with Allylic Phenoxides. A Simple Route 1,4-Alkadienes from Alkynes via Hydroboration$^\dag$

  • Sasaya Fumihito;Norio Miyaura;Akira Suzuki
    • Bulletin of the Korean Chemical Society
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    • v.8 no.4
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    • pp.329-332
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    • 1987
  • The reaction of (E)-1-alkenyl-1,3,2-benzodioxaboroles with a variety of allylic phenoxides in the presence of a catalytic amount of Pd$(PPh_3)_4$ is described. The reaction affords a general and simple procedure for the preparation of 1,4-alkadienes from alkynes via hydroboration.

Isolation and Structure of cis,fac -Dibromooxotris(2,6-dimethylphenyl isocyanide)molybdenum(IV), cis,fac-$[Mo(O)Br_2(CN-C_6H_3-2,6-Me_2)_3]$ (cis,fac-Dibromooxotris(2,6- dimethylphenyl isocyanide)molybdenum (IV), cis,fac-$[Mo(O)Br_2(CN-C_6H_3-2,6-Me_2)_3]$의 분리 및 구조)

  • 이범준;한원석;이순원
    • Korean Journal of Crystallography
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    • v.13 no.2
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    • pp.82-85
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    • 2002
  • From the reaction of cis,cis,trans- [MoBr/sub 2/(CO)/sub 2/(PPh/sub 3/)/sub 2/]with 2,6-dimethylphenyl isocyanide, a molybdenum oxohaloisocyanide compound cis,fac-[Mo(O)Br/sub 2/,(CN-C/sub 6/H/sub 3/,-2,6-Me/sub 2/)sub 3/] (1) was iso-lated. Compound 1 was characterized by spectroscopy (/sup 1/H-NMR, /sup 13/C{/sup 1/H}-NMR, IR) and X-ray diffraction. Crystallographic data for 1: triclinic space group P(equation omitted), a=9.172(2) (equation omitted), b = 11.550(3) (equation omitted), c = 15.106(3) (equation omitted), α = 100.44(2)°, β= 107.12(2)°, γ= 107.83(1)°, Z = 2, R(wR/sub 2/) = 0.0529(0.1344).

Synthesis and Characterization of Homo-, Hetero-Dinuclear Mo(Ⅲ) and V(Ⅲ) Complexes (Ⅳ) (몰리브덴(Ⅲ) 과 바나듐(Ⅲ) 호모 및 헤테로 이핵 착물의 합성과 특성 (제 4 보))

  • O, Sang O;Yu, Eun Yeong
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.808-818
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    • 1994
  • The neutral compounds [$MCl_3L_2$(MeCN)] (M = Mo, V: L = $PPh_3$, 1/2 phda) have been prepared from the reaction of starting material $MCl_z$ (M = Mo; z = 5, M = V; z = 3) with N,P-donating ligands in acetonitrile solution. Addition of $AgClO_4$ to these neutral monomeric compounds in acetone solution were produced [$MCl_3-_nL_2(MeCN)(S)_n$]$(ClO_4)_n$ (n = 1, 2 : s = solvent). Finally treatment of bivalent cationic compound and neutral compound was formed chloride bridged dinuclear complex $[(MeCN)(L)_2ClM({\mu}-Cl)_2M'Cl(L)_2(MeCN)](ClO_4)_2$ and treatment of univalent cationic compound with half equivalent pyrazine to pyrazine bridged complex $[(MeCN)(L)_2Cl_2M({\mu}-pyz)M'Cl_2(L)_2(MeCN)](ClO_4)_2$. These complexes are characterized by elemental analysis, $^1H$, $^{13}C$ NMR, IR, Far-IR and UV-Vis spectroscopy.

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Synthesis and Structure of trans-Bis[bis(diphenylphosphino)ethane]cyanohydridoiron(II), trans[FeH(CN)$(dppe)_2$](dppe=$Ph_2PCH_2CH_2PPh_2)$ ([FeH(CN)$(dppe)_2$ 착물의 합성 및 구조)

  • 이재경;최남선;이순원
    • Korean Journal of Crystallography
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    • v.10 no.1
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    • pp.45-50
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    • 1999
  • Ar 기류하에서 trans-[FeH(NCCH2CH2CH2Cl)(dppe)2][BF4], 1과 KCN이 반응하여 trans-[FeH(CN)(dppe)2], 2가 생성되었다. 이 화합물의 구조가 NMR, IR, 원소분석, 그리고 X-ray 회절법으로 규명되었다. 착물 2의 결정학 자료: 단사정계 공간군 p21/c, a=13.580(1) b=20.178(2) , c=17.592(3) , β=92.22(1)o, Z=4,(wR2)=0.0659(0.1692).

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Evaluation of L-FMUS as a potent anti-HBV agent

  • Woo, Seong-Ju;Lee, Hae-Sung;Cheong, Min-Young;Ahn, Kwang-Hyun;Park, Ki-Seok;Koo, Chang-Hui
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.242.1-242.1
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    • 2003
  • The nucleoside analogue, L-FMUS was synthesized from L-FMAU which has been shown to have significant antiviral activity against hepatitis B virus (HBV). It was prepared by two steps. First, 5'hydroxyl of L-FMAU was substituted by thioacetyl group using diisopropylazodicarboxylate(DIAD), Triphenyl phosphine(PPh3) and thioacetic acid in anhydrous THF. (omitted)

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