Primary and secondary trimethylsilylmethylstibines. Synthesis, characterization and chemical vapor deposition properties
摘要:
The primary and secondary trimethylsilylmethylstibines (trimethylsilylmethyl = Me3SiCH2-) (Me3SiCH2)SbH2 and (Me3SiCH2)2SbH have been synthesized by the reduction of a corresponding dihalo- and monohaloantimony compound, respectively. Trimethylsilylmethylstibine was prepared by the reduction of (Me3SiCH2)SbBr2 With lithium aluminum hydride (LAH) in tetraglyme. The primary stibine is highly air-sensitive and exhibits a vapor pressure of 2.0 Torr at 0-degrees-C. Bis-(trimethytsilylmethyl)stibine was synthesized by the LAH reduction of either (Me3SiCH2)2SbBr or (Me3SiCH2)2SbI in diethyl ether, The secondary stibine is less sensitive to air than (Me3SiCH2)SbH2 but nonetheless decomposes quickly when exposed to air. The detailed synthesis, spectroscopic characterizations and physical properties of both stibines, as well as the preliminary chemical vapor deposition experiments of (Me3SiCH2)SbH2, are discussed.