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1.4-Dibora-2,5-cyclohexadiene 유도체를 리간드로 갖는 니켈 Double-decker 착물의 합성
엄재국,Eom, Jae Guk 대한화학회 2002 대한화학회지 Vol.46 No.3
(${\eta}^5$-Cyclopentadienyl)(${\eta}^6$-1,2,3,4-tetramethyl-1,4-dibora-2,5-cyclohexadiene)Ni(5)는 cyclopentadienyl (carbonyl)-nickel dimer와 1,2,3,4-tetramethyl-1,4-dibora-2-cyclohexene (1)을 반응시켜서 주생성물로 얻었다. Di-allyl nickel과 2,3-diethyl-1,4-dimethyl-1,4-dibora-2-cyclohexene (2)을 -20$^{\circ}C$에서 반응시켜서 bis[${\eta}^6$-2,3-dimethyl-1,4-diethoxy-1,4-dibora-2,5-cyclohexadiene]nickel (6) 착화합물을 15% 수율로 생성하였다. 그리고 야-allyl nickel과 2,3-dimethyl-1,4-diethoxy-1,4-dibora-2-cyclohexene (3)을 역시 -20$^{\circ}C$에서 반응시켜서 22% 수율로 bis[${\eta}^6$-2,3-dimethyl-1,4-diethoxy-1,4-dibora-2,5-cyclohexadiene] nickel (7)을 생성하였다. 이들 double-decker 착화합물들은 불안정하여 분리하기 어려웠으며, NMR, MS, 원소분석 등으로 확인하였다. (${\eta}$5-Cyclopentadienyl)(${\eta}$6-1,2,3,4-tetramethyl-1,4-dibora-2,5-cyclohexadiene)Ni (5) was synthe-sizedas a main product by the reaction of cyclopentadienyl(carbonyl)nickel dimer and 1,2,3,4-tetramethyl-1,4-di-bora-2-cyclohexene (1). Di-allyl nickel reacted with 2,3-diethyl-1,4-di-methyl-1,4-dibora-2-cyclohexene (2) at -20$^{\circ}C$ to give bis(${\eta}$6-2,3-diethyl- 1,4-dimethyl-1,4-dibora-2,5-cyclohexadiene)nickel (6) in the yield of 15%. By the reaction of di-allyl nickel and 2,3-dimethyl-1,4-diethoxy-1,4-di- bora-2-cyclohexene (3) at -20$^{\circ}C$ bis[${\eta}$6-2,3-dim-ethyl-1,4-diethoxy-1,4-di- bora-2,5-cyclohexadiene]nickel (7) was obtained in 22% yield. These double-decker complexes were difficult to separate because of their unstabilities and were identified by ESR, NMR, MS and ele-mental analysis, etc.
엄재국,박영배,변상인,이혁,곽영우,김태정,Uhm Jae-Kook,Park Young-Bae,Byun Sang-In,Lee Hyuk,Kwak Young-Woo,Kim Tae-Jeong 대한화학회 1991 대한화학회지 Vol.35 No.4
트리플 데카 착물, bis(${\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.
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.
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.