Synthesis and deprotonation of (phenylselenolatodimethylsilyl)bis(trimethylsilyl) methane: The crystal structure of (Meb>3b>Si)b>2b>(Meb>2b>SiBr)CH

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• 作者：Sushil K. Gupta^a ; ^{skggwr@gmail.com} ; Sujata Yumnam^a ; Peter B. Hitchcock^b
• 关键词：Synthesis ; Bromodimethylsilylbis(trimethylsilyl)methane ; Bulky selenium containing silicon ligand ; Lithium derivative ; NMR spectra ; X-ray structure
• 刊名：Journal of Molecular Structure
• 出版年：2012
• 期刊代码：62_00222860
• 类别：ch
• 出版时间：27 June, 2012
• 卷：1018
• 期：Complete
• 页码：137-144
• 文件大小：952 K

摘要

The moisture-sensitive compound [{bromodimethylsilyl}bis(trimethylsilyl)methane], [(Meb>3b>Si)b>2b>(Meb>2b>SiBr)CH] boldFont">1 has been synthesized by the bromination of the hydride [(Meb>3b>Si)b>2b>(Meb>2b>SiH)CH] in CClb>4b> in good yield. Compound boldFont">1 has been characterized by multinuclear NMR and a single crystal X-ray diffraction studies. The average Si-C and BrMeb>2b>Si-C distances are, respectively, 1.894(2) and 1.886(2) 脜. The Si-C-Si angle is 114.98(13)掳. Treatment of boldFont">1 with NaSePh (obtained from the sodium triethylborohydride reduction of diphenyldiselenide) in benzene at room temperature resulted in the isolation of light yellow oil, [{phenylselenatodimethylsilyl}bis(trimethylsilyl)methane], [(Meb>3b>Si)b>2b>(Meb>2b>SiSePh)CH] boldFont">2. Compound boldFont">2 has been metallated with methyllithium as well as lithium diisopropylamide (LDA) in THF to give [(Meb>3b>Si)b>2b>(Meb>2b>SiSePh)CLi路2THF] boldFont">3. Compounds boldFont">2 and boldFont">3 have been characterized by elemental analysis, mass and multinuclear NMR studies.