Divalent platinum complex and preparation method and application thereof
A platinum complex, complex technology, applied in platinum group organic compounds, platinum group organic compounds, chemical instruments and methods, etc.
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Embodiment 1
[0069] Embodiment 1 Complex 2 and its preparation
[0070] Synthesis of 2-((6-bromo-4-(1H-pyrazol-1-yl)pyridin-2-yl)oxy)-9-(pyridin-2-yl)-9H-carbazole:
[0071]
[0072] To a sealed 75 mL tube with a magnetic rotor was added 2,6-dibromo-4-(1H-pyrazol-1-yl)pyridine (2.11 g, 7 mmol), 9-(2-pyridyl)-9H-carb Azol-2-ol (1.65g, 6.36mmol), N,N-dimethylglycine (526mg, 5.1mmol), cuprous iodide (121mg, 0.636mmol), cesium carbonate (5.21g, 16mmol) and 1, 4-Dioxane (25 mL), the resulting mixture was bubbled with nitrogen for 10 minutes and then heated to 120° C. and stirred for 48 hours. Cool to room temperature, add water to quench the reaction, extract with ethyl acetate, combine the organic phases, wash with an appropriate amount of saturated aqueous sodium chloride solution and dry over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude product was separated and purified by silica gel column chromatography, and the eluent was pet...
Embodiment 2
[0082] Embodiment 2 Complex 3 and its preparation
[0083] Synthesis of 2-((6-isobutyl-4-(1H-pyrazol-1-yl)pyridin-2-yl)oxy)-9-(pyridin-2-yl)-9H-carbazole L3:
[0084]
[0085] To a sealed 5 mL tube with a magnetic rotor was added 2-((6-bromo-4-(1H-pyrazol-1-yl)pyridin-2-yl)oxy)-9-(pyridin-2-yl) -9H-carbazole (241mg, 0.5mmol), isobutylboronic acid (102mg, 1mmol), tetrakistriphenylphosphopalladium (18mg, 0.015mmol), potassium phosphate (200mg, 0.75mmol) and toluene (5mL), to obtain The mixture was bubbled with nitrogen for 10 min and then heated to 100 °C and stirred overnight. Cool to room temperature, add water to quench the reaction, extract with ethyl acetate, combine the organic phases, wash with an appropriate amount of saturated aqueous sodium chloride solution and dry over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude product was separated and purified by silica gel column chromatography, the eluent was petrol...
Embodiment 3
[0089] Embodiment 3 Complex 4 and its preparation
[0090] Synthesis of 2-((6-trimethylphenyl-4-(1H-pyrazol-1-yl)pyridin-2-yl)oxy)-9-(pyridin-2-yl)-9H-carbazole L4:
[0091]
[0092] To a sealed 5 mL tube with a magnetic rotor was added 2-((6-bromo-4-(1H-pyrazol-1-yl)pyridin-2-yl)oxy)-9-(pyridin-2-yl) -9H-carbazole (168mg, 0.35mmol), 2,4,6-trimethylphenylboronic acid (115mg, 0.7mmol), tris(dibenzylideneacetone) dipalladium (10mg, 0.0105mmol), tricyclohexyl Phosphine (4mg, 0.014mmol), cesium carbonate (228mg, 0.7mmol) and dioxane (1mL), the resulting mixture was bubbled with nitrogen for 10 minutes and then heated to 80°C and stirred overnight. Cool to room temperature, add water to quench the reaction, extract with ethyl acetate, combine the organic phases, wash with an appropriate amount of saturated aqueous sodium chloride solution, and dry over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude product was separated a...
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