Syntheses of a stable tristibine and of related antimony compounds with the 2,6-dimesitylphenyl (Dmp) substituent

DmpSbBr2 (Dmp = 2,6-Mes2C6H3) (1) is obtained by the reaction of DmpMgBr with SbCl3. The reaction of 1 with KI in ethanol gives DmpSbI2 (2). Dmp(Ph)SbBr (3) is prepared from DmpMgBr and PhSbCl2. Compound 1 or 3 react with LiAlH4 to form DmpSbH2 (4) or Dmp(Ph)SbH (5). Compound 4 reacts with MeI in presence of DBU to give Dmp(Me)SbH (6). DmpSb(SbMe2)2 (7) is obtained from 4 and Me4Sb2. Elimination of hydrogen from 6 gives [Dmp(Me)Sb]2 (8). Hydrolysis of 3 gives Dmp(Ph)SbOH (9). The molecular structures of 1–3, 5, 8 and 9 were determined by X-ray diffraction on single crystals.