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엄재국 啓明大學校 生活科學硏究所 1980 科學論集 Vol.6 No.-
Dioximes were synthesized via diones or dialdehydes with hydroxyl amine. Their structures were investigated by means of NMR spectroscopy. The conformer of Glyoxal dioxime was found to have the perfect symmetric structure, “syn-syn” form. The conformers of 2,5-hexandione dioxime were found to have the mixture of “syn-syn” and “syn-anti”forms. The configuration of Methyl glyoxal dioxime was investigated from the “anisotropic effect”of -OH group, that is, to have “syn-anti”form.
엄재국,박영배,변상인,이혁,곽영우,김태정,Uhm Jae-Kook,Park Young-Bae,Byun Sang-In,Lee Hyuk,Kwak Young-Woo,Kim Tae-Jeong 대한화학회 1991 대한화학회지 Vol.35 No.4
트리플 데카 착물, bis(${\eta}^5$-cyclopentadienyl)-${\mu}$-(${\eta}^6$-2,3-dialkyl-1,4-dimethyl-1,4-dibora-2,5-cyclohexadiene)dicobalt 1을 합성하고, 이것을 출발물질로 하여 여기에 3-hexyne을 과량으로 반응시켰더니 두 종류의 sandwich 착물인 cyclopentadienyl(${\eta}^6$-2,3-dialkyl-1,4-dimethyl-1,4-dibora-2,5-cyclohexadiene)cobalt 2와 cyclopentadienyl(${\eta}^6$-hexaethyl benzene)cobalt 3가 분리되었다. 착물 3은 실온에서 정제하는 동안 분해하여 3-hexyne의 고리화 반응 생성물인 hexaethyl benzene이 생성되었음을 확인하였다. A tripledecker sandwichcomplex, bis(${\eta}^5$-cyclopentadienyl)-${\mu}$-(${\eta}^6$-2,3-dialkyl-1,4-dimethyl-1,4-dibora-2,5-cyclohexadiene)dicobalt 1 was synthesized as a starting material. By the reaction of compound 1 with the excess 3-hexyne two kinds of sandwichcomplexes, cyclopentadienyl(${\eta}^6$-2,3-dialkyl-1,4-dimethyl-1,4-dibora-2,5-cyclohexadiene)cobalt 2 and cyclopentadienyl(${\eta}^6$-hexaethyl benzene)cobalt 3 were separated. The complex 3 was decomposed during purifying at RT to give a cyclization product of 3-hexyne, hexaethyl benzene.
$C_2$ 손대칭 리간드를 배위하는 $\pi$-Allyl-Cobalt, Palladium, Platinum 착물의 생성
엄재국,이종오,안희원,Uhm, Jae Kook,Lee, Jong O,An, Hee Won 대한화학회 1998 대한화학회지 Vol.42 No.2
C2-손대칭 리간드(chiral ligand)의 한 종류인 (+)-11S,12S-bis [2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene과 백금과 코발트를 포함하는 착물과 각각 반응시켜, 세 종류의 새로운 착물인 $\pi$-allyl Pt(+)-11S,12S-bis[2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene perchlorate, $\pi$-allyl Pt(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene chloride, (${\eta}$5-cyclopentadienyl) Co -(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene를 얻었다. 그리고 (${\eta}$3-cyclohexenyl) Pd 착물과 대칭리간드인 1,2-bis(diphenylphosphino)ethane 과 반응시켜 새로운 착물, (${\eta}$3-cyclohexenyl) Pd1,2-bis(diphenylphosphino)ethane perchlorate를 생성하였다. 이들 착물은 NMR-, IR-, Mass-spectrometer, 원소분석등의 각종 화학분석기기에 의해 각각 확인되었다. By the reactions of a $C_{2}$-chiral ligand, (+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene(6) with $[\pi-allyl chloroplatinum(II)]_4$, and $CpCo(CO)_2$ respectively, three new complexes, ($\pi$-allyl)platinum(II)(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene perchlorate(1), ($\pi$-allyl)platinum(II)(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene chloride(2), ($\eta^5$-cyclopentadienyl)cobalt(I)-(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene(3) were prepared. $\eta^3$-Cyclohexenyl)palladium(II)1,2-bis(diphenylphosphino)ethane perchlorate(4) was obtained by the reaction of ($\eta^3$-cyclohexenyl)palladium(II) chloride dimer with a symmetric ligand, 1,2-bis(diphenylphosphino)ethane and lithium perchlorate. These complexes were identified by NMR-, IR-, and Mass-Spectrophotometers and elemental analyzer.
Tripledecker 착물, $(CpCo)_2(C_4R_4)$과 Alkyne과의 반응
엄재국,이원식,김석봉,차진순,이형수,이동호,김홍석,심상철,Uhm, Jae-Kook,Lee, Won-Sik,Kim, Seog-Bong,Cha, Jin-Soon,Lee, Hyung-Soo,Lee, Dong-Ho,Kim, Hong-Seok,Sim, Sang-Chul 대한화학회 1993 대한화학회지 Vol.37 No.9
트리플데카 착물류, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraalkylcyclobutadiene$)dicobalt들은 Jonas 시약과 2-hexyne 또는 3-hexyne을 실온에서 동량으로 반응시킬 때, 50% 이상의 최대 수율이 얻어졌다. 한 종류의 트리플데카 착물인 bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraethyl cyclobutadiene$)dicobalt(13)는 실온에서 3-hexyne과 반응시키면, 착물 (${\eta}^5-cyclopentadienyl)cobaltacyclopentadiene-{\mu}-({\eta}^4-2,4-cobaltacyclopentadiene$)(${\eta}^5-cyclopentadienyl$)cobalt(15)로 이성화되었다. 다른 한 종류의 트리플데카 착물, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,3-dimethyl-2,4-dipropyl cyclobutadiene$)dicobalt(14)를 2-hexyne과 반응시켰더니 1,3,5-trimethyl-2,4,6-tripropylbenzene 화합물이 생성되었다. The tripledecker complexes, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraalkylcyclobutadiene$)dicobalt were produced by the reaction of Jonas reagent with 2-hexyne and 3-hexyne in the maximum yield (above 50%) when they were reacted in eq-molar amounts at room temperature. A tripledecker complex, bis-${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraethyl cyclobutadiene$)dicobalt(13) was isomerized to (${\eta}^5-cyclopentadienyl)cobaltacyclopentadiene-{\mu}-({\eta}^4-2,4-cobaltacyclopentadiene$)(${\eta}^5-cyclopentadienyl$)cobalt(15) on reacting with 3-hexyne at room temperature. Another tripledecker complex, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,3-dimethyl-2,4-dipropyl cyclobutadiene$)dicobalt(14) was decomposed to give 1,3,5-trimethyl-2,4,6-tripropylbenzene through an intermediate complex by the reaction of 2-hexyne.
1,2,3,4,5,6-Hexaalkyl-1,4-dibora-2-cyclohexene의 생성과 착물 생성
엄재국,안희원,Uhm, Jae-Koouk,An, Hee-Won 대한화학회 1997 대한화학회지 Vol.41 No.11
1,2,3,4,5,6-hexaalkyl-1,4-dibora-2-cyclohexene은 $B_2Cl_4$로부터 제조할 수 있었으나, 보통실험실에서는 이것을 제조하기 어렵기 때문에 다른 방법에 의한 생성을 시도하였다. 즉,1,4-dimethyl-2,3-diethyl-1,4-dibora-2-cyclohexene, 1 유도체를 potassium과 methyl iodide에 의한 환원${\cdot}$산화반응을 시켜주므로 2,3-dietyl-1,4,5,6-tetramethyl-1,4-dibora-2-cyclohexene, 2를 얻을 수 있었다. 또 이 유도체와 ($({\eta}5-C_5H_5Co(C_2H_4)_2$를 반응시켜 코발트 sandwich 착물인 두 종류의 double-decker, 6 그리고 7, 또 한 종류의 triple-decker, 8을 생성하였다. 1,2,3,4,5,6-Hexaalkyl-1,4-dibora-2-cyclohexene was not produced by the general preparation method in our laboratory because of difficulties in the preparation of $B_2Cl_4.$ 2,3-Dietyl-1,4,5,6-tetramethyl-1,4-dibora-2-cyclohexene, 2 was synthesized by the reduction-oxidation reaction of potassium and methyliodide from 1,4-dimethyl-2,3-diethyl-1,4-dibora-2-cyclohexene, 1 as a substrate. Cobalt sandwich-complexes, 6, 7 and 8 were synthesized by the reaction of 2,3-diethyl-1,4,5,6-tetramethyl-1,4-dibora-2-cyclohexene with $({\eta}5-C_5H_5Co(C_2H_4)_2.$.