40°C. Slow warm-up to room temperature, column chromatographic work-up (silica gel flash chromatography, elution with a 10 : 1 : 1 mixture of dichloromethane, petroleum ether (30-50°C) and diethyl ether), and Kugelrohr distillation (bath temperature 45 "C at 0.1 torr) afforded the a-methylene-p-lact
Cleavage of the Fe–Fe Bond of (Me2SiSiMe2)[η5-C5H4Fe (CO)2]2 with Na/Hg and Molecular Structure of the Ring-Opened Complex
✍ Scribed by Hud-Lin Sun; Zhen-Sheng Zhang; Xiu-Zhong Zhou
- Publisher
- John Wiley and Sons
- Year
- 2010
- Tongue
- English
- Weight
- 327 KB
- Volume
- 21
- Category
- Article
- ISSN
- 0256-7660
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✦ Synopsis
Abstract
The reaction of the title cyclic complex (1) with sodium amalgam in THF resulted in the expected cleavage of the Fe—Fe bond to afford bis‐sodium salt (Me~2~SiSiMe~2~) [η^5^‐C~5~H~4~Fe (CO)~2~Na]~2~ (4). The latter was not isolated and was used directly to react with MeI, PhCH~2~Cl, CH~3~C(O)Cl, PhC(O)Cl, Cy~3~SnCl (Cy = cyclohexyl) or Ph~3~SnCl to afford corresponding ring‐opened derivatives (Me~2~SiSiMe~2~) [η5‐C~5~H~4~Fe (CO)~3~R]~2~ [5, R=Me; 6, R = PhCH~2~; 7, R = CH~3~C(O); 8, R = PhC (O); 9, R = Cy~3~Sn or 10, R = Ph~3~Sn]. The crystal and molecular structures of 10 were determined by X‐ray diffraction analysis. The molecule took the desired anti conformation around the Si—Si bond. The length of the Si—Si bond is 0.2343(3) nm, which is essentially identical to that in the cyclic structure of 1 [0.2346(4) nm]. This result unambiguously demonstrates that the Si—Si bond in the cyclic structure of 1 is not subject to obvious ring strain.
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Metallocenes / P ligands /