The synthesis and characterization of a barium silyl-phosphide by a low temperature route
| Autor: | Phillip Hall, Simon R. Drake, Roger Lincoln |
|---|---|
| Rok vydání: | 1993 |
| Předmět: |
Addition reaction
Silylation Phosphide Inorganic chemistry chemistry.chemical_element Barium Nuclear magnetic resonance spectroscopy Sodium hydride Inorganic Chemistry chemistry.chemical_compound chemistry Materials Chemistry Physical and Theoretical Chemistry Tetramethylsilane Phosphine Nuclear chemistry |
| Zdroj: | Polyhedron. 12:2307-2311 |
| ISSN: | 0277-5387 |
| Popis: | The reaction of tetramethylsilane and sodium hydride in a mixed solvent of THF and HMPA (2:1 by volume), at reflux for 40 h, followed by the addition of PCl 3 yielded (Me 3 Si) 3 ( 1 ) in excellent yield by a simple, non-hazardous and facile route. This phosphine was readily converted into the known phosphide (Me 3 Si) 2 PH ( 2 ) by controlled hydrolysis. Reaction of this ligand with barium granules in a mixed liquid ammonia-THF solvent system at −40°C yielded the first barium silylphosphide, [Ba(P{SiMe 3 } 2 ) 2 (THF) 2 ] n ( 3 , which was characterized by IR, 1 H, 13 C and 29 Si NMR spectroscopy. |
| Databáze: | OpenAIRE |
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