N,O-single ligand metal catalyst with stereochemical structure and preparation method thereof
A metal catalyst and three-dimensional structure technology, applied in the direction of organic chemistry, etc., can solve the problems of poor tolerance and low activity of polar monomers, and achieve the effects of low dielectric constant, high light transmittance, and good thermal stability.
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Embodiment 1
[0040] (I) Preparation of α-ketophenylimine ligands with three-dimensional structure.
[0041] Add 0.0143 mol of 9,10-dihydro-9,10-ethylene anthracene-11,12-dione, 0.0143 mol of aniline, and a catalytic amount of p-toluene into the reaction flask equipped with a reflux condenser and a water separator Sulfonic acid and 150 mL of toluene were used as solvents. After reacting for 2 hours, the novel stereoscopic α-ketobenimine ligand with a purity of more than 99% was obtained by recrystallization from n-hexane or distillation under reduced pressure.
[0042] (II) Preparation of mono(α-ketophenylimine)nickel(II) with three-dimensional structure of the main catalyst.
[0043] -78 o C slowly add the solution of n-butyllithium dissolved in toluene and n-hexane to the toluene containing the ligand prepared in step I, and the molar ratio of the two is 1:1. Then wait for the temperature of the mixture to slowly return to room temperature, and stir for 2 h. Then add 1 equivalent of t...
Embodiment 2
[0047] (I) Preparation of α-ketophenylimine ligands with three-dimensional structure.
[0048] With embodiment 1.
[0049] (II) Preparation of mono(α-ketophenylimine)palladium(II) complexes with the stereostructure of the main catalyst.
[0050] -78 o C slowly add the solution of n-butyllithium dissolved in toluene and n-hexane to the toluene containing the ligand prepared in step I, the molar ratio of the two is 1:1. Then wait for the temperature of the mixture to slowly return to room temperature, and stir for 2 h. Then add 1 equivalent of trans-[Pd(PPh 3 ) 2 (Ph)Cl]. Stir continuously overnight at room temperature, filter, and recrystallize to obtain a mono(α-ketophenylimine)palladium(II) complex with a new stereostructure.
[0051] (III) Catalytic polymerization of norbornene.
[0052] Heat the reaction bottle equipped with a magnetic stirrer and a branch with a heat gun, and simultaneously vacuumize it, fill it with nitrogen, and replace it three times to ensure th...
Embodiment 3
[0054] (I) Preparation of α-keto(2,6-dimethyl)phenylimine ligand with three-dimensional structure.
[0055] Add 0.0143 mol of 9,10-dihydro-9,10-ethylene anthracene-11,12-dione, 0.0143 mol of 2,6-dimethyl Aniline, a catalytic amount of p-toluenesulfonic acid and 200 mL of toluene were used as solvents. After reacting for 4 hours, recrystallize with n-hexane or distill under reduced pressure to obtain the α-keto(2,6-dimethyl)phenylimine ligand with a purity of more than 99%.
[0056] (II) Preparation of mono[α-keto(2,6-dimethyl)phenylimine]nickel(II) complex with stereostructure of procatalyst.
[0057] -78 o C slowly add the solution of n-butyllithium dissolved in toluene and n-hexane to the toluene containing the ligand prepared in step I, the molar ratio of the two is 1:1. Then wait for the temperature of the mixture to slowly return to room temperature, and stir for 2 h. Then add 1 equivalent of trans-[Ni(PPh 3 ) 2 (Ph)Cl]. Stir continuously overnight at room temperat...
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