[N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and preparation method and application thereof
A technology of metal complexes and tetradentate ligands, which is applied in the fields of compounds of group 4/14 elements of the periodic table, titanium organic compounds, chemical instruments and methods, etc., which can solve the problems of high cost, complex catalyst structure, and many synthesis steps, etc. problem, to achieve the effect of long life, stable structure and high catalytic activity
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Embodiment 1
[0034] Example 1 Type I tetradentate ligand L 11 Preparation of H2
[0035]
[0036] Under the condition of stirring at -78°C, add 10ml of a hexane solution of n-butyllithium with a concentration of 2mol / L to 20ml of a tetrahydrofuran solution of o-phenylenediamine with a concentration of 0.5mol / L, and naturally rise to room temperature to react 2 Hours, a tetrahydrofuran solution of lithium o-phenylenediamide was obtained. The tetrahydrofuran solution of lithium o-phenylenediamide was added to 20 ml of the 1 mol / L compound A tetrahydrofuran solution, and the reaction was stirred at 50° C. for 2 hours. The temperature of the reaction solution was lowered to -78°C, and 5 ml of n-butyllithium hexane solution with a concentration of 2 mol / L was added, and the reaction solution was allowed to rise to room temperature naturally, and then stirred overnight. The solvent tetrahydrofuran was distilled off, the product was extracted with dichloromethane and water, the organic phase...
Embodiment 2
[0037] Example 2 Type I tetradentate ligand L 12 Preparation of H2
[0038]
[0039] Under the condition of stirring at -78°C, add 10ml of a hexane solution of n-butyllithium with a concentration of 2mol / L to 20ml of a tetrahydrofuran solution of o-phenylenediamine with a concentration of 0.5mol / L, and naturally rise to room temperature to react 2 Hours, a tetrahydrofuran solution of lithium o-phenylenediamide was obtained. The tetrahydrofuran solution of lithium o-phenylenediamide was added to 20 ml of the 1 mol / L compound B tetrahydrofuran solution, and the reaction was stirred at 50° C. for 2 hours. The temperature of the reaction solution was lowered to -78°C, and 5 ml of n-butyllithium hexane solution with a concentration of 2 mol / L was added, and the reaction solution was allowed to rise to room temperature naturally, and then stirred overnight. The solvent tetrahydrofuran was distilled off, the product was extracted with dichloromethane and water, the organic phase...
Embodiment 3
[0040] Example 3 Type II tetradentate ligand L 21 Preparation of H2.
[0041]
[0042] Under the condition of stirring at room temperature, o-phenylenediamine (0.54g, 5.0mmol), compound C (2.25g, 10.0mmol) and p-toluenesulfonic acid (0.10g) were mixed in 20ml of toluene, and the water separator was used to reflux for 10 After 1 hour, the reaction solution was cooled to room temperature, the solvent toluene was distilled off, and column chromatography was carried out using petroleum ether / ethyl acetate for separation or recrystallization in petroleum ether / ethyl acetate solvent to obtain 2.11 g of a light yellow solid pure product with a yield of 81%. , denoted as tetradentate ligand L 21 H2.
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