Organic iridium metal complex as well as preparation method and application thereof
An iridium metal complex, organic technology, applied in indium organic compounds, platinum group organic compounds, organic chemistry, etc.
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Embodiment 1
[0078] Preparation of Compound F001
[0079]
[0080] (1) Under nitrogen protection system, weigh A-001 (66.35mmol, 20g), IrCl 3 ·3H 2 O (22.12mmol, 7.8g) was added to the reaction system, a mixed solution of 600mL ethylene glycol ether and 200mL purified water was added, refluxed for 24 hours under the protection of nitrogen, and then cooled to room temperature, a precipitate was precipitated, and the precipitate was filtered with water, The bridging ligand B-001 (11.2 g, yield 61.12%) was obtained as a red powder by washing and drying with absolute ethanol and petroleum ether in sequence.
[0081] (2) Under the nitrogen protection system, weigh B-001 (6.76mmol, 11.2g), C-001 (20.28mmol, 2.03g), and then add 250mL of ethylene glycol ether and potassium carbonate (67.59mmol, 9.34g), under the protection of nitrogen, stirred at 120°C for 24 hours, suction filtered, washed with alcohol, dried, and used dichloromethane as solvent, followed by silica gel column chromatography...
Embodiment 2
[0088] Preparation of Compound F010
[0089]
[0090] (1) Under nitrogen protection system, weigh A-010 (37.04mmol, 20g), IrCl 3 ·3H 2 O (12.35mmol, 4.35g) was added to the reaction system, a mixed solution of 600mL ethylene glycol ether and 200mL purified water was added, refluxed for 24 hours under the protection of nitrogen, and then cooled to room temperature, a precipitate was precipitated, and the precipitate was filtered with water, The bridging ligand B-010 (10.4 g, yield 64.52%) was obtained as a red powder by washing and drying with absolute ethanol and petroleum ether in sequence.
[0091] (2) Under nitrogen protection system, weigh B-010 (3.98mmol, 10.4g), add C-010 (11.95mmol, 1.2g), then add ethylene glycol ethyl ether 250mL and potassium carbonate (39.83mmol , 5.51g), under the protection of nitrogen, stirred at 120°C for 24 hours, suction filtered, washed with alcohol, dried, and used dichloromethane as a solvent, followed by silica gel column chromatograp...
Embodiment 3
[0096] Preparation of Compound F012
[0097]
[0098] (1) Under nitrogen protection system, weigh A-012 (56.42mmol, 20g), IrCl 3 ·3H 2 O (18.81mmol, 6.63g) was put into the reaction system, a mixed solution of 600mL ethylene glycol ether and 200mL pure water was added, refluxed for 24 hours under the protection of nitrogen, and then cooled to room temperature, a precipitate was precipitated, the precipitate was suction filtered, and water , absolute ethanol, and petroleum ether were washed and dried in turn to obtain a red powder of bridging ligand B-012 (5.72 g, yield 60.88%).
[0099] (2) Under nitrogen protection system, weigh B-012 (5.72mmol, 10.7g), add C-012 (17.17mmol, 1.721g), then add ethylene glycol ethyl ether 250mL and potassium carbonate (57.24mmol , 7.91g), under the protection of nitrogen, stirred at 120°C for 24 hours, suction filtered, washed with alcohol, dried, used dichloromethane as solvent, and used silica gel column chromatography, the filtrate was ...
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