摘要
A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YC13 with CF3CH2ONa in a 1 : 3 molar ratio in THF at room temperature, after workup, gave complex 1 as colorless crystals. The composition of complex 1 is [Y(OCH2CF3)3]6ONa2(THF)12, which was identified by elemental analysis and ^1H NMR. Further X-ray structure determination reveals that complex 1 is a polynuclear ion pair compound, [Y6(μ6-O)(OCH2CF3)18]^2- [Na(THF)6]2+ (1). The crystal data of complex 1 are trigonal, P-3 space group, a = 1.78440(14) nm, b = 1.78440(14) nm, c = 1.27395(12) nm, γ= 120°, V=3.5129(5) nm^3, Z = 1, Dc = 1.607 mg·m^-3, μ = 2.591 mm^- 1(Mo Ka), F(000) = 1710, R = 0.067, wR = 0. 182. Preliminary results demonstrated that complex 1 is a highly effective catalyst for the oligomerization of phenyl isocyanate.
A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YC13 with CF3CH2ONa in a 1 : 3 molar ratio in THF at room temperature, after workup, gave complex 1 as colorless crystals. The composition of complex 1 is [Y(OCH2CF3)3]6ONa2(THF)12, which was identified by elemental analysis and ^1H NMR. Further X-ray structure determination reveals that complex 1 is a polynuclear ion pair compound, [Y6(μ6-O)(OCH2CF3)18]^2- [Na(THF)6]2+ (1). The crystal data of complex 1 are trigonal, P-3 space group, a = 1.78440(14) nm, b = 1.78440(14) nm, c = 1.27395(12) nm, γ= 120°, V=3.5129(5) nm^3, Z = 1, Dc = 1.607 mg·m^-3, μ = 2.591 mm^- 1(Mo Ka), F(000) = 1710, R = 0.067, wR = 0. 182. Preliminary results demonstrated that complex 1 is a highly effective catalyst for the oligomerization of phenyl isocyanate.
基金
Project supported bythe National Natural Science Foundation of China (20472063)