Microwave‐Assisted Generation of Lanthanide(II) Halides in THF and Simple Quantitative Determination

作者: Anders Dahlén , Göran Hilmersson

DOI: 10.1002/EJIC.200400309

关键词:

摘要: Lanthanide(II) reagents (SmI2, SmBr2, YbI2, EuI2) have been prepared rapidly in high yields using microwave-assisted heating. Samarium diiodide is obtained as a saturated solution THF (0.13 M) within 5 min and ytterbium (0.065 after 45 min. A simple method for quantitative determination of LnX2 also described by utilizing the instantaneous reaction with ketones presence an amine water. This establishes concentration active single-electron-donor species, i.e. Ln2+. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)

参考文章(22)
Gary A. Molander, Samarium(II) Mediated Radical Reactions Radicals in Organic Synthesis. pp. 153- 182 ,(2008) , 10.1002/9783527618293.CH9
José M. Concellón, Humberto Rodríguez-Solla, Eva Bardales, Mónica Huerta, Very Rapid Preparation of SmI2 by Sonic Treatment of Iodoform and Metallic Samarium European Journal of Organic Chemistry. ,vol. 2003, pp. 1775- 1778 ,(2003) , 10.1002/EJOC.200210669
Brian W. Knettle, Robert A. Flowers, Influence of HMPA on reducing power and reactivity of SmBr(2). Organic Letters. ,vol. 3, pp. 2321- 2324 ,(2001) , 10.1021/OL0160957
Akiya Ogawa, Syoji Ohya, Yukihito Sumino, Noboru Sonoda, Toshikazu Hirao, Novel enhancement of the reducing ability of ytterbium diiodide by irradiation with near-UV light Tetrahedron Letters. ,vol. 38, pp. 9017- 9018 ,(1997) , 10.1016/S0040-4039(97)10409-9
Anders Dahlén, Göran Hilmersson, Instantaneous SmI2–H2O-mediated reduction of dialkyl ketones induced by amines in THF Tetrahedron Letters. ,vol. 43, pp. 7197- 7200 ,(2002) , 10.1016/S0040-4039(02)01673-8
William J. Evans, Donald K. Drummond, Hongming Zhang, Jerry L. Atwood, Synthesis and x-ray crystal structure of the divalent [bis(trimethylsilyl)amido] samarium complexes [(Me3Si)2N]2Sm(THF)2 and {[(Me3Si)2N]Sm(.mu.-I)(DME)(THF)}2 Inorganic Chemistry. ,vol. 27, pp. 575- 579 ,(1988) , 10.1021/IC00276A027
Gary A. Molander, Application of lanthanide reagents in organic synthesis Chemical Reviews. ,vol. 92, pp. 29- 68 ,(1992) , 10.1021/CR00009A002