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박유철,김경채,조영제,Park Yu-Chul,Kim Kyung-Chae,Cho Young-Jae 대한화학회 1992 대한화학회지 Vol.36 No.5
디포스핀을 포함한 몇가지 $d^8$ 전이금속착물$(MCl_2PP)$은 출발물질 $K_nMCl_m$을 사용하여 합성하였다. 중심금속(M)은 Ni(II), Pd(II), Pt(II), Au(III)이며, 디포스핀(PP)은 bis(diphenylphosphino)methane(dppm), bis(diphenylphosphino)ethane(dppe), bis(diphenylphosphino)propane (dppp) 및 bis(diphenylphosphino)ethylene(dppety)이었다. 착물의 조성이나 특성은 원소분석과 $^1H-NMR$, $^{31}P-NMR$ 및 UV-Visible 스펙트럼을 이용하여 확인하였다. 이들 착물의 촉매적 활성은 3(2H)-furanone 및 cyclic carbonate 생성반응에 대하여 각각 조사하였다. 2-methyl-3-butyn-2-ol로부터 생성물 3(2H)-furanone을 얻은 반응 (1)에서 Ni(II)-, Pd(II)-diphosphine 착물은 좋은 촉매적 효과를 나타내었다. 그러나 이들 diphosphine 착물들은 cyclic carbonate 생성반응 (2)에 대해 촉매제로서의 활성을 거의 나타내지 않았다. The $d^8$-transition metal complexes containing diphosphine, $MCl_2PP$ were prepared by using $K_nMCl_m$ as starting materials, wherein M were Ni(II), Pd(II), Pt(II) and Au(III) and PP were bis(diphenylphosphino)methane(dppm), bis(diphenylphosphino)ethane(dppe), bis(diphenylphosphino)propane (dppp) and bis(diphenylphosphino)ethylene(dppety). The complexes were characterized by the spectral property $(^H-NMR$, $^{31}P-NMR$ and UV-Visible spectra) together with elemental analysis. The complexes were tested for the catalytic activity on the formation reactions of 3(2H)-furanone and cyclic carbonate. The only Ni(II)- and Pd(II)-diphosphine complexes displayed a good catalytic effects in the production of 3(2H)-furanone from 2-methyl-3-butyn-2-ol [reaction (1)]. But all the diphosphine complexes as catalyst were almost inactive towards cyclic carbonate production preaction [reaction (2)].
Ni(2)-및 Cu(2)-dieneN4 거대고리착물의 합성과 분광학적 성질
박유철,김경채,조연하 경북대학교 환경과학연구소 1996 環境科學硏究所論文集 Vol.10 No.1
The tetra-aza macrocyclic ligand. 1.5,6.8.12.13-hexamethyl-1.4.8.11-tetraazacyclotetradeca-4.11-diene(C), was prepared as its dihydroperchlorate salt by the non-template condensation of 3-methyl-3-buten-2-one with N-methylethylenediamine. The Ni(II) and Cu(II) complexes of C were obtained by the reaction of its metal salts and C. These complexes were identified by the elemental analysis. iH(13C)-NMR. IR. and UV-vis. spectroscopy. Based on the result of NMR spectrum, it was found that this complex might be N-meso. The axial ligation of nitrogenous base(imidazole) to the Ni(II)-(A. B, C) complexes were investigated in nitromethane. The equilibrium constants for the ligation reactions of nickel complexes were determined using the spectrophotometric method at 15-45 C . In case of Ni(II)-A complex the equilibrium constants K were larger than Ni(II)-B and C complexes, depending on basicity of the ligand nitrogen.