A kind of aryl primary amine ruthenium complex, preparation method and use thereof
A technology for complexes and compounds, which is applied in the field of preparation of transition metal complexes, aryl primary amine ruthenium complexes, and can solve the problems of expensive raw materials, cumbersome preparation, and complex structures.
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Embodiment 1
[0068] Embodiment 1: [(n 6 -p-cymene) RuCl 2 (NH 2 -C 6 h 4 -p-CH 2 CN)] synthesis
[0069] (1) Weigh 2mmol ruthenium trichloride trihydrate (RuCl 3 ·3H 2 (2) and 10mmol p-cymene were put into a 50mL round bottom flask, 30ml absolute ethanol was added, and heated to reflux under nitrogen protection for 24 hours. After the reaction, cool to room temperature, filter, wash the solid with absolute ethanol, and dry in vacuo to obtain a brown solid, i.e. p-cymene dichloride ruthenium dimer, with a yield of 90%. The reaction formula is as follows:
[0070]
[0071] (2) Weigh 0.04 mmol of p-cymene ruthenium dichloride dimer and 0.1 mmol of 4-aminophenylacetonitrile into a 25 mL round bottom flask, add 10 mL of anhydrous methanol, and heat to reflux for 6 hours under nitrogen protection. After the reaction, cool to room temperature, filter, wash the solid with anhydrous methanol three times, and dry in vacuo to obtain a solid product with a yield of 92%.
[0072] Then take ...
Embodiment 2
[0077] Embodiment 2: [(n 6 -p-cymene) RuCl 2 (NH 2 -C 6 h 4 -p-NO 2 )]Synthesis
[0078] (1) Weigh 2mmol ruthenium trichloride trihydrate (RuCl 3 ·3H 2 O) and 20mmol p-cymene were put into a 50mL round-bottomed flask, 30ml THF was added, and heated to reflux under nitrogen protection for 10 hours. After the reaction was finished, cool to room temperature, filter, wash the solid with absolute ethanol, and dry in vacuo to obtain a brown solid, i.e. p-cymene dichloride ruthenium dimer, with a yield of 92%, and the reaction formula is the same as in Example 1 Step (1).
[0079] (2) Weigh 0.04 mmol p-cymene ruthenium dichloride dimer and 0.08 mmol 4-nitroaniline into a 25 mL round bottom flask, add 20 ml acetone, and heat to reflux for 24 hours under nitrogen protection. After the reaction, cool to room temperature, filter, wash the solid with anhydrous methanol three times, and dry in vacuo to obtain a solid product with a yield of 89%.
[0080] Then take this solid prod...
Embodiment 3
[0085] Embodiment 3: [(n 6 -p-cymene) RuCl 2 (NH 2 -C 6 h 4 -p-COOC 2 h 5 )]Synthesis
[0086] (1) Weigh 2mmol ruthenium trichloride (RuCl 3 ) and 15mmol p-cymene were put into a 50mL round-bottomed flask, 30ml ether was added, and heated to reflux under nitrogen protection for 15 hours. After the reaction was finished, cool to room temperature, filter, wash the solid with absolute ethanol, and dry in vacuo to obtain a brown solid, i.e. p-cymene dichloride ruthenium dimer, with a yield of 94%, and the reaction formula is the same as in Example 1 Step (1).
[0087] (2) Weigh 0.04 mmol p-cymene ruthenium dichloride dimer and 0.06 mmol 4-urethane into a 25 mL round bottom flask, add 20 ml toluene, and heat to reflux for 20 hours under nitrogen protection. After the reaction, cool to room temperature, filter, wash the solid with anhydrous methanol three times, and dry in vacuo to obtain a solid product with a yield of 85%.
[0088] Then take by weighing this solid produc...
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