247076-38-6Relevant articles and documents
Synthesis and Chemistry of Bis(borylphosphino)silanes and -germanes
Chen, Tuqiang,Duesler, Eileen N.,Paine, Robert T.,Noeth, Heinrich
, p. 4993 - 4999 (2008/10/08)
The reactions of Me2SiCl2, Ph2SiCl2, and Ph2GeCl2 with LiP(H)B(N(i)Pr2)2in a 1:2 ratio and the reaction of Ph2SiCl2 with LiP(H)B(N(i)Pr2)[N(SiM e3)2] in a 1:2 ratio give good yields of the respective diphosphinosilanes, Me2Si[P(H)B(N(i)Pr2)2]2, Ph2Si[P(H)B(N(i)Pr2)2]2, Ph2Ge[P(H)B(N(i)Pr2)2]2, and Ph2Si[P(H)B(N(i)Pr2)[N(SiMe3)2]]2. These species, when combined with BuLi in a 1:2 ratio, give lithium diphosphinosilanes and -germanes of the general type (DME.Li)2{[PB(NR2)2]2ER'2}. All of the species have been characterized by spectroscopic methods. The molecular structuresof three of the lithio compounds, (DME.Li)2{[PB(N(i)Pr2)2]2SiPh2} (11), (DME.Li)2{[PB(N(i)Pr2)N(SiMe3)2]2SiPh2} (15), and (DME.Li)2{[PB(N(i)Pr2 )2]2GePh2} (13), have been determined by X-ray diffraction techniques. 11 crystallized in the triclinic space group P1- with a = 11.071(2) ?, b = 14.937(3) ?, c = 18.080(4) ?, α = 91.31(3)°, β = 101.23(3)°, γ = 109.95(3)°, and Z = 2, and 13 crystallized in the triclinic space group P1- with a = 11.083(1) ?, b = 14.978(2) ?, c = 18.134(2) ?, α = 91.17(1)°,β = 101.43(1)°, γ = 110.05(1)°, and Z = 2. 15 crystallized in the monoclinic space group P21/n with a = 11.939(2) .ANG ., b = 24.516(3) ?, c = 21.572(3) ?, β = 101.52(1)°,and Z = 4. The reactions of the lithio compounds were surveyed with R2E Cl2 reagents. The metathesis reactions are sluggish, but the 1:1 reaction of (DME.Li)2{[PB(N(i)Pr2)2]2GePh2} with (t)Bu2SnCl2 gave the four-membered-ring compound Ph2GePB(N(i)Pr2)2Sn((t)Bu)2PB(N(i)Pr2)2. The 1:2 reaction of Me2(Cl)SiSi(Cl)Me2 with LiP(H)B(N(i)Pr2)2 yielded the (borylphosphino)silane [Me2SiP(H)B(N(i)Pr2)2]2.
