1310554-25-6Relevant academic research and scientific papers
On the reduction of NC chelated organoantimony(III) chlorides
Dostal, Libor,Jambor, Roman,Ruzicka, Ales,Simon, Petr
, p. 2380 - 2386 (2011)
The conversion of organolithium compound LLi, for which L = [o-C 6H4(CH=NC6H3iPr2-2,6)] -, with antimony chloride gave the molecular chlorides LSbCl 2 (1) and L2SbCl (2) depending on the molar ratio used (either 1:1 or 2:1). Bothcompounds were characterized by using 1H and 13C NMR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The reaction of 1 with two molar equivalents of K[B(sBu) 3H] led to smooth formation of compound L4Sb4 (3) as a result of hydrogen elimination from the unstable hydrido compound. On the contrary, a similar reaction between 2 and K[B(sBu)3H] (1:1) did not result in hydrogen elimination and the formation of expected distibine L2SbSbL2, but an addition of an in situ generated L 2Sb-H bond across the C=N functionality in the pendant arm of one of the ligands was observed. The reduction of compound 2 with an excess amount of magnesium was strongly dependent on the reaction time. The distibine L 2SbSbL2 (5) could be isolated after 4-5 h from this reaction mixture. Elongation of the reaction time to 1 d (and more) gave a more complicated reaction mixture, in which three products, distibine 5, compound 3 and organomagnesium compound L2Mg(THF) (6), were characterized by single-crystal X-ray diffraction in addition to other unidentified products. These results can be rationalized by a migration of the ligand L from the antimony atom to the magnesium, thus explaining formation of both L 4Sb4 (3) compound and L2Mg(THF) (6).
