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題名 | Preparations and 2D-HetCOR NMR Spectra of (η[fec3]-Carbomethoxycy clopentadienyl) Dicarbonylcobalt, Dicarbonyl (η[fec3]-N-Methyl-Carbamoylcy clopentadienyl) Cobalt and Dicarbonyl (η[fec3]-N-Phenyl-Carbamoyl cyclopentadienyl) Cobalt=[η[fec3]-(甲氧醯基)-環戊二烯]二羰鈷, [η[fec3]-(N-甲醯胺基)-環戊二烯]二羰鈷及[η[fec3]-(N-苯醯胺基)-環戊二烯〕二羰鈷之製備及光譜 |
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作者姓名(中文) | 王玉蘋; 林傳宗; | 書刊名 | 東海學報 |
卷期 | 34 1993.06[民82.06] |
頁次 | 頁683-699 |
分類號 | 341.393 |
關鍵詞 | η[fec3]-環戊二烯二羰鈷; 2D-HetCOR核磁光譜; Cyclopentadieny ldicarbonylcobalt; 2D-HetCOR spectrum; |
語文 | 英文(English) |
中文摘要 | 在四氫伕喃(THF)溶液中,環戊二醯基鈉鹽與碳酸二甲酯(dimethyl carbonate)反應生成[η��-(甲氧醯基)-環戊二桸]鈉鹽12。在四氫伕喃溶液中,12 與八羰二鈷及碘之混合物反應可生成[η��-(甲氧醯基)-環戊二烯]二羰鈷13,產率 為42%。在乙醇水溶液中,13與氫氧化鉀作用後酸化可得[η��-(羧酸基)-環戊二烯] 二羰鈷16,產率為74%。在苯溶液中,16與氯化乙二醯(oxylyl chloride)反應 生成[η��-(氯化醯基)-環戊二烯]二羰鈷17,產率為67%。17可與甲胺 (methylamine)及苯胺(aniline)分別作用產生N-甲醯胺14及苯醯胺15。在�螻B 及�C碳之核磁共振光譜中,化合物13-15的Cp(Co)環上H(2-5)及C(2-5)之化學 位移可利用2D-HetCOR核磁光譜儀技術確定之。 |
英文摘要 | A reaction between sodium cyclopentadienide and dimethyl carbonate in THF solution produces sodium carbomethoxycyclopentadienide 12 in high yield. Reaction of 12 with mixtures of octacarbonyldicobalt and iodime in THF solution affords (η�� - carbomethoxycyclopentadienyl)dicarbonylcobalt 13, in 42% yield. (η�� - Carboxycyclopentadienyl)dicarbonylcobalt 16 is obtained in 74% yield by treatment of ester 13 with potassium hydroxidein aqueous ethanol followed by acidification. A reaction between acid 16 and oxalyl chloide in benzene solution produces (η�� - chloroformylcyclopentadienyl)dicarbonylcobalt 17, in67% yield, and the latter reacts readily with methylamine and with aniline to form the respective N-methylamide 14 and anilide 15. The chemical shifts of H(2-5) protons and (2-5) carbons of Cpring in �� H and �C C NMR spectra, respectively, has been assigned unequivocally using 2D- HetCOR NMR spectroscopy for compounds13-15. |
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