A kind of aryl substituted pyridinium amine iron-based catalyst and its preparation method and application
A technology of pyridinium amine iron series and pyridinium amine iron, which is applied in the preparation of catalysts and the application of isoprene polymerization. In the field of pyridinium amine iron series catalysts, it can solve the problem of unclear active center of catalyst structure, low molecular weight of synthetic polymer, Poor selectivity and other issues, to achieve the effect of low cost, good industrial value, and high tolerance
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Embodiment 1
[0030] The present embodiment prepares the pyridine imine iron complex shown in formula (A):
[0031] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 and isopropyl substituted pyridine imine ligand (1.5 mmol) (structural formula LA), stirred at room temperature for 24 h. After the reaction, the dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain an off-white solid, structural formula:
[0032]
[0033] Mass Spectrometry: C 12 h 12 Cl 2 FeN 2 :[M-Cl] + : Theoretical value: 275.0033; measured value: 275.0042.
[0034] Elemental Analysis: C 12 h 12 Cl 2 FeN 2 : Theoretical value: C, 46.35; H, 3.89; N, 9.01; Measured value: C, 46.41%; H, 3.85%; N, 8.98%.
Embodiment 2
[0036] The preparation process of the pyridinium iron complex shown in formula (B) prepared in this embodiment is as follows:
[0037] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 and tert-butyl-substituted pyridinimine ligand (1.5 mmol) (structural formula LB), and stirred at room temperature for 24 h. After the reaction, the dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain a light blue solid with the structural formula:
[0038]
[0039] Mass Spectrometry: C 18 h 24 Cl 2 FeN 2 [M-Cl] + : Theoretical value: 359.0972; measured value: 359.0968.
[0040] Elemental Analysis: C 18 h 24 Cl 2 FeN 2 : Theoretical value: C, 54.71; H, 6.12; N, 7.09; Measured value: C, 54.68%; H, 6.09%; N, 7.13%.
Embodiment 3
[0042] The pyridine imine iron complex shown in the formula (C) prepared in this embodiment, the preparation process is as follows:
[0043] The 10mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, anhydrous FeCl 2 and cyclohexyl-substituted pyridine imine ligand (1.5 mmol) (structural formula LC), and stirred at room temperature for 48 h. After the reaction, the dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain a light red solid, structural formula:
[0044]
[0045] Mass Spectrometry: C 38 h 32 Cl 2 FeN 2 [M-Cl]+ : Theoretical value: 607.1598; measured value: 607.1601.
[0046] Elemental Analysis: C 38 h 32 Cl 2 FeN 2 : Theoretical value: C, 70.93; H, 5.01; N, 4.35; Measured value: C, 71.01%; H, 4.98%; N, 4.30%.
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