Bivalent rare earth complex containing pyridine substituted indene ligand and its use
A rare earth metal and complex technology, applied in the field of rare earth metal coordination compounds, can solve the problem of no catalytic activity and achieve the effect of large molecular weight, narrow molecular weight distribution and high syndiotactic content
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Embodiment 1
[0036] In an ice-water bath, 67 mL of n-BuLi (1.55 M, 104 mmol) in hexane was slowly added dropwise to a solution of indene (12 mL, 104 mmol) in 120 mL of tetrahydrofuran. The solution turned orange and was slowly warmed to room temperature and stirred overnight. Then the reaction mixture was introduced into the 3-(ClCH 2 )C 5 h 4 N.HCl (10.2g, 62mmol) was suspended in THF milky white candle, stirred for 12 hours. Then 50 mL of water was added to the solution, the inorganic layer was extracted with 2×15 mL of ether, the organic phases were combined, and dried with anhydrous MgSO4, the solvent was removed in vacuo, and 3-(3-pyridylmethyl)indene was obtained by distillation under reduced pressure. Elemental analysis result (%): calculated value: (C 15 h 13 N): C, 86.92; H, 6.32; N, 6.67. Found values: C, 86.18; H, 6.23; N, 6.65
Embodiment 2
[0038] In 50mL of toluene solution containing 3-(3-pyridylmethyl)indene (0.49g, 2.38mmol), add [(Me 3 Si) 2 N] 3 Yb III (μ-Cl)Li(THF) 3 (1.09g, 1.19mmol), the reaction mixture was stirred overnight at room temperature, then heated (about 80°C) for 12 hours, and the solvent was removed to obtain a dark green solid, which was washed with 10mL of n-hexane, and then washed with 10.0mL×2 hot The product was extracted with THF. The filtrates were combined and concentrated to about 10 mL. After standing at 0°C for several days, 0.64 g of dark green powder bis[(3-(3-pyridyl)indenyl)ytterbium was obtained with a yield of 71%. Elemental analysis result (%): calculated value: (C 30 h 24 N 2 Yb·C 7 h 8 ): C, 65.57; H, 4.76; N, 4.13. Found: C, 65.10; H, 4.65; N, 4.58.
Embodiment 3
[0040] In 50mL of toluene solution containing 3-(3-pyridylmethyl)indene (0.45g, 2.18mmol), add [(Me 3 Si) 2 N] 3 Eu III (μ-Cl)Li(THF) 3 (0.96g, 1.09mmol), the reaction mixture was stirred overnight at room temperature, then heated (about 50°C) for 12 hours, and the solvent was removed to obtain a dark green solid, which was washed with 10mL of n-hexane and then washed with 10.0mL×2 hot The product was extracted with THF. The filtrates were combined and concentrated to about 10 mL. Stand several days at 0 ℃, obtain dark green powder two ((3-(3-pyridyl) indenyl) europium 0.46g, productive rate 65%. Elemental analysis result (%): calculated value (C 30 h 24 N 2 Eu): C, 63.83; H, 4.30; N, 4.96. Found: C, 64.43; H, 4.95; N, 4.35.
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