206538-84-3Relevant articles and documents
Reactions of Phosphoric Acid Triesters with Aluminum and Gallium Amides
Pinkas, Jiri,Wessel, Helge,Yang, Yu,Montero, Mavis L.,Noltemeyer, Mathias,Froeba, Michael,Roesky, Herbert W.
, p. 2450 - 2457 (2008/10/08)
Triesters of phosphoric acid OP(OR)3 (R = Me, Et, n-Bu, SiMe3) react with [M(NMe2)3]2 (M = Al (1), Ga (2)) in nonaqueous aprotic solvents with the formation of amorphous alumino- and gallophosphates MPO4 (M = Al, Ga). Triphenyl phosphate, on the other hand, undergoes ligand scrambling with 1 and 2. Aluminophosphate also results from the reaction of AlCl3 with OP(OSiMe3)3. The products and mechanisms of these reactions were examined by 1H, 13C, 29Si, and 31P NMR spectroscopy, X-ray powder diffraction (XRD), thermogravimetric methods (TG/DTA), infrared spectroscopy (IR), and elemental analyses. The molecular structure of the first-step model compound (Me2N)3Al·OPPh3 (3) was established by the single-crystal X-ray diffraction experiment. Crystal data for 3 (-70 °C): a = 8.870(2) A, b = 10.195(3) A, c = 14.706(5) A, α = 90.27(3)°, β = 94.04(2)°, γ = 109.61(2)°, V = 1249.0(6) A3, Z = 2, triclinic space group P1 (No. 2). Alumazene [MeAlNDipp]3 (4) forms a bis-adduct [MeAlNDipp]3·2OP(OMe)3 (5) with trimethyl phosphate. The molecular structure of 5 was also elucidated by X-ray crystallography. Crystal data for 5 (-140 °C): a = 12.176(2) A, b = 12.630(3) A, c = 21.376(4) A, α = 96.04(3)°, β = 90.46(3)°, γ = 115.38(3)°, V = 2948(1) A3, Z = 2, triclinic space group P1 (No. 2).
