Synthesis and Characterization of A Polynuclear Yttrium Trifluoroethoxide and Its Activity for Oligomerization of Phenyl Isocyanate
来源期刊:JOURNAL OF RARE EARTHS2006年第4期
论文作者:Deng Mingyu Zhang Yong Shen Qi Peng Hongmei Yao Yingming
Key words:inorganic chemistry; lanthanide alkoxo complex; trifluoroethoxide; crystal structure; rare earths;
Abstract: A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YCl3 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) nm3, Z=1, Dc=1.607 mg·m-3, μ=2.591 mm-1 (Mo Kα), 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.
Deng Mingyu1,Zhang Yong1,Shen Qi1,Peng Hongmei1,Yao Yingming1
(1.Key Laboratory of Organic Synthesis of Jiangsu Province, Department of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215123, China)
Abstract:A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YCl3 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) nm3, Z=1, Dc=1.607 mg·m-3, μ=2.591 mm-1 (Mo Kα), 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.
Key words:inorganic chemistry; lanthanide alkoxo complex; trifluoroethoxide; crystal structure; rare earths;
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