Preparation and application of carborane benzothiazole ligand containing semi-sandwich iridium complex
A technology of benzothiazole and iridium complexes, applied in the field of semi-sandwich iridium complexes and their preparation, can solve the problems of poor stability, harsh preparation and storage conditions, etc., and achieve high stability, excellent selectivity, stable physical and chemical properties Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0024] Example 1: Synthesis of half-sandwich iridium complexes containing carborane benzothiazole ligands
[0025]
[0026] At –78°C, n-BuLi (1.6M) n-hexane solution (1.00mL, 1.6mmol) was slowly added dropwise to the ortho carborane o-C 2 B 10 h 10 (92.0mg, 0.64mmol) in tetrahydrofuran solution, continue stirring at this temperature for 30 minutes after the dropwise addition, slowly rise to room temperature and continue the reaction for 1 hour, then add bromobenzothiazole (137.0mg, 0.64mmol), continue The reaction was carried out at room temperature for 6 hours. Then the binuclear iridium compound [Cp*IrCl 2 ] 2 (256.0 mg, 0.32 mmol) was added to the reaction system for another 3 hours. After the reaction is finished, stand and filter, and dry the solvent under reduced pressure, and the obtained crude product is subjected to column chromatography separation (petroleum ether / tetrahydrofuran=6:1) to obtain the red target product, the carborane shown in formula (I) Half-...
Embodiment 2
[0029] Embodiment 2: catalytic ethylene polymerization reaction
[0030] The semi-sandwich iridium complex (i.e. catalyst Ir) containing the carborane benzothiazole ligand shown in the formula (I) prepared in Example 1 is used to catalyze ethylene polymerization: under anhydrous and oxygen-free conditions, in a reaction vessel Add 1mL of half-sandwich iridium catalyst in chlorobenzene solution (0.1 μmol), MAO in toluene solution 0.19mL (300 μmol), the ratio of the amount of semi-sandwich iridium complex to MAO is 1:3000, and ethylene gas is introduced at normal pressure , the gas flow rate is 6mL / s, the ethylene polymerization reaction is carried out under anhydrous and oxygen-free conditions, the reaction temperature is 30 ° C, after 15 minutes of reaction, the reaction is terminated with an ethanol solution containing 10% hydrochloric acid by volume, and the resulting product is filtered and used Wash with ethanol several times, and dry in vacuum at 60-80°C until the quality...
Embodiment 3
[0031] Embodiment 3: catalytic ethylene polymerization reaction
[0032] The semi-sandwich iridium complex (i.e. catalyst Ir) containing the carborane benzothiazole ligand shown in the formula (I) prepared in Example 1 is used to catalyze ethylene polymerization: under anhydrous and oxygen-free conditions, in a reaction vessel Add the chlorobenzene solution (0.5 μ mol) of 5mL semi-sandwich iridium catalyst successively, the toluene solution 0.32mL (500 μ mol) of MAO, the ratio of the amount of substance of catalyst Ir and MAO is 1:1000, and normal pressure feeds ethylene gas, gas flow rate 6mL / s, carry out ethylene polymerization reaction under anhydrous and oxygen-free conditions, the reaction temperature is 30 ℃, after 15 minutes of reaction, stop the reaction with ethanol solution containing 10% hydrochloric acid by volume, filter the obtained product, and wash several times with ethanol The second time, vacuum-dry at 60-80°C until the quality remains unchanged. The activi...
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com