Chiral pyridine bis-imidazole ligand transition metal complex catalyst and preparation method thereof
A technology of pyridine bis-imidazole and transition metal, which is applied in the field of chiral pyridine bis-imidazole ligand transition metal complex catalyst and its preparation, can solve the problems of expensive ligands and difficult synthesis, and achieve cheap and easy-to-obtain raw materials. The effect of simple synthesis operation and mild reaction conditions
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Embodiment 1
[0039] Embodiment 1: prepare chiral pyridine bis-imidazole ligand-iron complex 1a of the present invention, its structural formula is:
[0040]
[0041] In the glove box, the FeCl 2 (126.8 mg, 1.0 mmol, 1.0 equiv) and THF (50 mL) were added to a 100 mL schlenk tube, and then a THF solution (10 mL ) was added dropwise to the above solution, and at the moment of addition, the color of the reaction solution rapidly changed to purple-black, and a purple-black solid was precipitated. After the reaction was stirred at room temperature for 24 h, it was filtered, washed with THF and ether, and the solvent was drained to obtain a purple-black powder (1.02 g, 87%). Then put the above powder (15 mg) into a sample bottle with a volume of 4 mL, dissolve it in DMSO (1 mL), transfer the above sample bottle to a sample bottle with a volume of 18 mL containing ether solvent, and the ether solvent cannot cover Small sample vial mouth, let it stand for several days, wait for the diethyl et...
Embodiment 2
[0042] Embodiment 2: Preparation of chiral pyridine bis-imidazole ligand-iron complex [(NNN) of the present invention 2 Fe] 2+ FeCl 4 2- (complex 1b), its structural formula is:
[0043]
[0044] In the glove box, the FeCl 2 (126.8 mg, 1.0 mmol, 1.0 equiv) and THF (50 mL) were added to a 100 mL schlenk tube, and then a THF solution (10 mL ) was added dropwise to the above solution, and at the moment of addition, the color of the reaction solution rapidly changed to purple-black, and a purple-black solid was precipitated. After the reaction was stirred at room temperature for 24 h, it was filtered, washed with THF and ether, and the solvent was drained to obtain a purple-black powder (583.1 mg, 83%). Anal. Calcd for C 78 h 74 Cl 4 Fe 2 N 10 : C, 66.68; H, 5.31; N, 9.97. Found: C, 67.06; H, 5.68; N, 10.26.
Embodiment 3
[0045] Embodiment 3: Preparation of chiral pyridine bis-imidazole ligand-iron complex [(NNN) of the present invention 2 Fe] 2+ Cl 2 2- (complex 1c), its structural formula is:
[0046]
[0047] In the glove box, the FeCl 2 (126.8 mg, 1.0 mmol, 1.0 equiv) and THF (50 mL) were added to a 100 mL schlenk tube, and then a THF solution (10 mL ) was added dropwise to the above solution, the color of the reaction solution rapidly changed to purple-black, and a purple-black solid was precipitated. After the reaction was stirred at room temperature for 24 h, it was filtered, washed with THF and ether, and the solvent was drained to obtain a purple-black powder (1.00 g, 81%). Anal. Calcd for C 70 h 56 Cl 4 FeN 10 : C, 68.08; H, 4.57; N, 11.54. Found: C,68.53; H, 4.91; N, 11.70.
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