一种合成[闭式-B12(OH)12]-2的改进方法。

An improved method for the synthesis of [closo-B12(OH)12]-2.

作者信息

Bayer Michael J, Hawthorne M Frederick

机构信息

Department of Chemistry and Biochemistry, University of California-Los Angeles, 607 Charles E. Young Drive East, Los Angeles, CA 90095-1569, USA.

出版信息

Inorg Chem. 2004 Mar 22;43(6):2018-20. doi: 10.1021/ic030289w.

DOI:10.1021/ic030289w

PMID:15018524

Abstract

The dicesium salt of the icosahedral borane anion dodecahydroxy-closo-dodecaborate(2-), closo-Cs(2)B(12)(OH)(12), Cs(2)4, was prepared using an improved synthetic pathway. Heating cesium dodecahydro-closo-dodecaborate, closo-Cs(2)B(12)H(12), Cs(2)1, with 30% hydrogen peroxide added in successive increments at 105-110 degrees C provided Cs(2)4 in 95% yield. Reaction progress was monitored using (1)H-decoupled (11)B NMR while (17)O NMR provides the most reliable way to detect the presence of peroxides in the reaction solution. The reaction may be safely increased in scale to afford Cs(2)4 in multigram quantities.

摘要

利用改进的合成路线制备了二十面体硼烷阴离子十二羟基-闭式-十二硼酸盐（2-），即闭式-Cs₂B₁₂(OH)₁₂，Cs₂4的铯盐。在105-110℃下，将十二氢-闭式-十二硼酸钾盐，闭式-Cs₂B₁₂H₁₂，Cs₂1，逐次增量加入30%的过氧化氢进行加热，以95%的产率得到Cs₂4。反应进程通过¹H去耦¹¹B NMR进行监测，而¹⁷O NMR提供了检测反应溶液中过氧化物存在的最可靠方法。该反应可以安全地扩大规模，以获得多克量的Cs₂4。