A kind of benzimidazole bisphosphine cu (i) complex and preparation method thereof
A technology of benzimidazole and complex, applied in the field of organic complex synthesis, can solve the problems of high price, hindering application, not abundant pollution and the like
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Embodiment 1
[0051](1) Add aniline (3.3 mL, 36.2 mmol), 2,6-diitropylbenzene (3 ml, 30 mmol) and no water supply (1.8 g, 30 mmol) to 9 ml dimethyl sulfoxide, stirring After dissolving, the reaction was 15 h at 95 ° C; after the reaction was completed, the system was cooled to room temperature, and then 30 ml of distilled water was added to the reaction system, stirred to a large amount of red precipitate, and precipitate filtered and washed 3 times with 30 ml (10 ml × 3 times). 3 times, Filtering the solid is dried in a dry box to obtain an intermediate product.
[0052] (2) The intermediates A (7 g, 20 mmol) obtained by step (1) and the intermediate dyldimeter (1.34 g, 10 mmol) were added to 120 ml of mixed solvent (the volume ratio of ethanol and water was 5: 1), stirred Dissolve, then adding sodium sulfite (20 g, 120 mmol), refluxed at 125 ° C for 8 h; after the reaction was completed, the system was cooled to room temperature, and the ethanol in the recovery system was completed, then the ...
Embodiment 2
[0056] (1) Add aniline (3.3 mL, 36.2 mmol), 2,6-diitropylbenzene (3 ml, 30 mmol) and no water supply (1.8 g, 30 mmol) to 9 ml dimethyl sulfoxide, stirring After dissolving, it was 100 ° C for 12 h; after the reaction was completed, the system was cooled to room temperature, and then 30 ml of distilled water was added to the reaction system, stirred to a large amount of red precipitation, filtered precipitate and washed 3 times with 30 mL (10 mL × 3 times). 3 times, Filtering the solid is dried in a dry box to obtain an intermediate product.
[0057] (2) The intermediates A (7 g, 20 mmol) obtained by step (1) and the intermediate dyldimeter (1.34 g, 10 mmol) were added to 120 ml of mixed solvent (the volume ratio of ethanol and water was 5: 1), stirred Dissolved, then adding sodium sulfite (20 g, 120 mmol), and refluxed at 130 ° C for 6 h; after the reaction was completed, the system was cooled to room temperature, and the ethanol in the recovery system was completed, then the orga...
Embodiment 3
[0061] (1) Add aniline (3.3 mL, 36.2 mmol), 2,6-diitropylbenzene (3 ml, 30 mmol) and no water supply (1.8 g, 30 mmol) to 9 ml dimethyl sulfoxide, stirring After the dissolution was complete, the system was reacted at 98 ° C for 14 h; after the reaction was completed, the system was cooled to room temperature, and then 30 ml of distilled water was added to the reaction system, stirred to a large amount of red precipitate, and precipitate and washed 3 times with 30 mL (10 mL × 3 times). 3 times, Filtering the solid is dried in a dry box to obtain an intermediate product.
[0062] (2) The intermediates A (7 g, 20 mmol) obtained by step (1) and the intermediate dyldimeter (1.34 g, 10 mmol) were added to 120 ml of mixed solvent (the volume ratio of ethanol and water was 5: 1), stirred Dissolve, then adding sodium sulfite (20 g, 120 mmol), refluxed at 128 ° C for 7 h; after the reaction was completed, the system was cooled to room temperature, and the ethanol in the recovery system was ...
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