A kind of carbon nanotube with Fe complex attached and its application
A technology of carbon nanotubes and complexes, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve the problem of using toxic solvents, harsh reaction conditions, and low yields Ideal and other issues, to achieve the effect of easy-to-obtain raw materials, mild synthesis reaction conditions, and low cost
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[0029]1) Preparation of Fe complex:
[0030]Weigh 0.4-0.8g FeCl3·6H2O, then add 10-20mL ethanol to a 50mL round-bottomed flask, add 0.2-0.5mL diamine compound dropwise using a constant pressure dropping funnel, and stir for 1-2h in an oil bath at 80°C. After the reaction, cool to room temperature, filter with suction, wash the filter cake with ethanol, and dry in vacuum;
[0031]2) Fe complexes are attached to carbon nanotubes:
[0032]Weigh 1-2g carbon nanotubes and 0.2-0.6g iron complex into a 50mL round bottom flask, add 10-20mL ethanol, stir at room temperature for 1-5h, then transfer to a sealed hydrothermal synthesis kettle, and place it in 100- Bake in an oven at 150°C for 1-2 days, then cool to 50-70°C for 12-20 hours. Finally, it is placed in a muffle furnace and baked at 180-250°C for 1-2 hours to obtain a carbon nanotube catalyst with Fe complexes.
Embodiment 1
[0034]
[0035]Weigh 1-phenyl-1,3-butanedione 2a (2mmol) and Fe complex-carrying carbon nanotube catalyst (150mg) in a 50mL Schlenk reaction flask, add 1,2-dichloride under air 20 mL of ethane and aniline 3a (4 mmol) were stirred at room temperature for 2 minutes, and then placed in an oil bath at 80°C to react for 12 hours. After the reaction, the mixture was cooled to room temperature, filtered through Celite, the filtrate was collected and the volatile components were removed under reduced pressure, and then separated by silica gel column chromatography (eluent was petroleum ether (60-90°C) / ethyl acetate) , V / v=20:1) to obtain the target product 1a (334mg, yield 70%) as a yellow solid. The target product was confirmed by nuclear magnetic resonance spectroscopy.
Embodiment 2
[0037]
[0038]Weigh 1-phenyl-1,3-butanedione 2a (2mmol) and Fe complex-carrying carbon nanotube catalyst (150mg) in a 50mL Schlenk reaction flask, add 1,2-dichloride under air 20 mL of ethane and p-toluidine 3b (4 mmol) were stirred at room temperature for 2 minutes, and then placed in an oil bath at 80°C to react for 12 hours. After the reaction, the mixture was cooled to room temperature, filtered through Celite, the filtrate was collected and the volatile components were removed under reduced pressure, and then separated by silica gel column chromatography (eluent was petroleum ether (60-90°C) / ethyl acetate) , V / v=20:1) to obtain the target product 1b (479mg, yield 95%) as a yellow solid. The target product was confirmed by nuclear magnetic resonance spectroscopy.
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