Synthese von Mesitylstibanen / Synthesis of Mesitylstibanes

Abstract

Trimesitylstibane (1) reacts with SbCl₃ or SbBr₃ to form the halostibanes Mes₂SbCl (2), MesSbCl₃ (3), Mes₂SbBr (4). or MesSbBr₂ (5) [Mes = 2,4,6-(CH₃)₃C₆H₂]. Action of MesMgCl on an excess of SbCl₃ or SbBr₃ at low temperatures gives Mes₃SbCl₂ (6) or Mes₃SbBr₂ (7), resp. Addi­tion of Br₂ to 1 gives 7 in 96% yield. The silylstibanes Mes₂SbSiMe₃ (8) and McsSb(SiMc₃)₂ (9) are formed by dehalogenation of Me₃SiCl and 4 or 5 by Mg filings in tetrahydrofuran. Mes₂SbOSiMe₃ (10) is obtained by air oxidation of 8. Reduction of 4 with Mg gives Mes₂SbSbMes₂ (19). Crystals of the composition (MesSb)₆·C₆H₆ (13a) or (MesSb)₄·C₆H₅CH₃ (13b) are obtained from Mg and 5 after work-up in benzene or toluene, resp.