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東海科學
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| 篇名 | 2D HETCOR NMR Spectra of (η5-1-carboethoxy-2-methylcyclopentadienyl)dicarbonylnitrosylchromium, (η5-1-carboethoxy-3-methylcyclopentadienyl)dicarbonylnitrosylchromium, and dicarbonyl(η5-1-carboxy-2-methylcyclopentadienyl)nitrosylchromium [η5-2-(CH3)C5H3COOR]Cr(CO)2(NO) ( R = H, C2H5) and [η5-3-(CH3)C5H3COOC2H5]Cr(CO)2(NO) |
|---|---|
| 卷期 | 17 |
| 並列篇名 | 錯合物CO)2(NO)Cr[η5-2-(CH3)C5H3COOR] (R=H,C2H5)及CO)2(NO)Cr[η5-3-(CH3)C5H3COOC2H5] 二維異核NMR光譜 |
| 作者 | 王玉蘋 、 廖仁海 |
| 頁次 | 010-025 |
| 關鍵字 | Chromium 、 cynichrodene 、 ferrocene 、 2D HETCOR-NMR 、 鉻 、 二碳 、 二茂鐵 、 TSCI |
| 出刊日期 | 201506 |
中文摘要
鈉塩Na+(η5-C5H4CH3)-與diethylcarbonate反應得雙取代Cp鈉塩sodium 1-carboethoxy-2-methylcyclopentadienide及sodium 1-carboethoxy-3-methylcyclopentadienide.加入Cr(CO)6,回流後 所得之metal carbonyl anion以乙酸酸化,可得hydrido錯化物[η5-2-(CH3)C5H3COOC2H5]Cr(CO)3(H)及[η5-3-(CH3)C5H3COOC2H5]Cr(CO)3(H).接下來以N-methyl-N-nitroso-p-toluenesulfonamide進行nitrosylation可得酯錯化物[η5-2-(CH3)C5H3COOCH3]CrCO)2(NO) 3及[η5-3-(CH3)C5H3COOCH3]CrCO)2(NO) 4.錯化物3經saponication(皂化反應)得錯化物酸[η5-2-(CH3)C5H3COOH]CrCO)2(NO) 5.藉由HETCOR NMR spectroscopy錯化物3－5Cp環上的 碳化學位移得以明確地標示出
英文摘要
Reaction of sodium methylcyclopentadienide with diethylcarbonate led to a mixture of sodium 1-carboethoxy-2-methylcyclopentadienide and sodium 1-carboethoxy-3-methylcyclopentadienide. After the mixture was refluxed with Cr(CO)6 in DMF, the metal carbonyl anion obtained was converted to the corresponding hydrido complexes [η5-2-(CH3)C5H3COOC2H5]Cr(CO)3(H) and [η5-3-(CH3)C5H3COOC2H5]Cr(CO)3(H), by adding acetic acid. A subsequent nitrosylation with N-methyl-N-nitroso-p-toluenesulfonamide gave the corresponding ester complexes 3 and 4. Chromium acid 5 was obtained after saponification of 3.The chemical shifts of C(2,5) and C(3,4) on the Cp ring of 3–5 have been assigned using two-dimensional HETCOR NMR spectroscopy.