Dinuclear half-sandwich iridium complex containing bisimine ligand and preparation method and application thereof
A technology of iridium complex and bis-imine, applied in the field of synthetic chemistry, can solve problems such as product yield decline, and achieve the effects of less by-products, high thermal stability and high yield
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[0022] Example 1: Synthesis of dinuclear semi-sandwich iridium complex containing bisimine ligand
[0023]
[0024] At -78°C, add n-BuLi (1.6M) in n-hexane solution (1.0 mL, 1.6 mmol) dropwise to the pyrrole ring bisimine ligand C 10 H 10 N 4 (119.0mg, 0.64mmol) in the tetrahydrofuran solution, after the dripping, continue to stir for 50 minutes, slowly rise to room temperature and continue the reaction for 60 minutes, then add pentamethylcyclopentadienyl iridium chloride dimer [Cp * IrCl 2 ] 2 (460.0mg, 0.58mmol), continue to react at room temperature for 4 hours; after the reaction is over, stand still and filter, and the solvent is drained under reduced pressure. The resulting crude product is separated by column chromatography (petroleum ether / dichloromethane (v / v )=6:1) Obtain the orange-red target product C 30 H 38 Cl 2 Ir 2 N 4 (437.0mg, yield 83%). The crystal structure diagram is as figure 1 Shown. Single crystal culture method: Dissolve 20 mg of the purified iridium com...
Example Embodiment
[0027] Example 2: Dinuclear semi-sandwich iridium complexes containing diimine ligands catalyze the oxidation of halogenated hydrocarbons to aldehydes
[0028]
[0029] Using the catalyst prepared in Example 1 to catalyze the oxidation reaction of halogenated hydrocarbons: To bromoethane (1mmol, 109mg) and adding a DMSO solution containing a binuclear semi-sandwich iridium complex (0.001mmol, 0.9mg), open reaction, reaction The temperature is 30°C and the reaction time is 270 minutes. After the reaction, the reaction solution is washed with water, extracted and concentrated. The crude product is separated by silica gel column chromatography and dried until the mass remains unchanged to obtain the corresponding aldehyde compound C 2 H 4 O (41 mg, yield 93%), elemental analysis: C 54.53, H 9.15 (theoretical); C 54.43, H 9.19 (actual).
Example Embodiment
[0030] Example 3: Dinuclear semi-sandwich iridium complex containing diimine ligand catalyzes the oxidation of halogenated hydrocarbons to aldehydes
[0031]
[0032] The catalyst prepared in Example 1 was used to catalyze the oxidation reaction of halogenated hydrocarbons: To chloropropane (1mmol, 80mg) was added a DMSO solution containing a binuclear half-sandwich iridium complex (0.001mmol, 0.9mg), open reaction, reaction temperature The reaction time is 300 minutes at 50°C. After the reaction, the reaction solution is washed with water, extracted and concentrated. The crude product is separated by silica gel column chromatography and dried until the quality remains unchanged to obtain the corresponding aldehyde compound C 3 H 6 O (55 mg, yield 95%), elemental analysis: C 62.04, H 10.41 (theoretical); C 62.03, H 10.53 (actual).
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