Iron complex and preparation method thereof, iron catalyst and application thereof, and polybutadiene and preparation method thereof
A technology of iron complexes and iron catalysts, applied in iron organic compounds, iron group organic compounds without C-metal bonds, etc., can solve the problems of low crystallinity, achieve fast polymerization reaction speed, simple and easy-to-operate preparation method, The effect of stable catalytic performance
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[0032] The second aspect of the present invention provides a method for preparing an iron complex, which is characterized in that the method comprises, under the conditions of a coordination reaction, combining a compound having a structure shown in formula (2) and a ferrous halide salt in a first organic contact in a solvent,
[0033]
[0034] Among them, R 1 , R 2 , R 3 , R 4 and R 5 The definition of and R in formula (1) 1 , R 2 , R 3 , R 4 and R 5 have the same definition.
[0035] According to the present invention, the amount of the compound having the structure shown in formula (2) and the ferrous halide salt can be varied within a wide range, as long as the iron complex with the structure shown in formula (1) can be formed. In order to obtain higher yields of iron complexes, preferably, the molar ratio of the compound having the structure shown in formula (2) to the ferrous halide salt is 1:0.9-1.1, more preferably 1:0.95- 1.
[0036] In the present inve...
preparation example 1
[0092] Under Ar atmosphere, the compound of the structure shown in 1mmol formula (3) (wherein, R 1 , R 2 and R 5 Each is independently hydrogen; the compound (R 3 and R 4 Each independently is methyl), sodium tert-butoxide (2.1mmol), toluene 5ml, bisdibenzylideneacetone palladium (0.052mmol), 2-dicyclohexylphosphino-2'-(N,N-dimethyl Amine)-biphenyl (0.10 mmol) was stirred at 110° C. for 4 hours. The resulting reaction solution was concentrated, and the mixture was subjected to SiO 2 Column chromatography, hexane / toluene=2:1 (volume ratio), obtains ligand L 1 . For ligand L 1 After analysis, the results are as follows:
[0093] L 1 , yield 70.5%. 1 H NMR (400MHz, CDCl 3 )δ2.36(s,6H,-CH 3 ), 4.12(br,1H,-NH),6.81-6.98(m,4H,Ar),7.19-7.35(m,7H,Ar),7.88(d,J=8.0Hz,1H,Ar),8.18( d, J=8.0 Hz, 1H, Ar), 8.45 (s, 1H, -N=CH).
preparation example 2
[0095] Under Ar atmosphere, the compound of the structure shown in 1mmol formula (3) (wherein, R 1 , R 2 Each independently is a methyl group, R 5 is hydrogen; the compound (R 3 and R 4 each independently hydrogen), sodium tert-butoxide (2.1 mmol), toluene 5 ml, bisdibenzylideneacetone palladium (0.052 mmol), 2-dicyclohexylphosphino-2'-(N,N-dimethylamine )-biphenyl (0.1 mmol) was stirred at 105°C for 5 hours. The resulting reaction solution was concentrated, and the mixture was subjected to SiO 2 Column chromatography, hexane / toluene=2:1 (volume ratio), obtains ligand L 2 . For ligand L 2 After analysis, the results are as follows:
[0096] L 2 , yield 72.1%. 1 H NMR (400MHz, CDCl 3 )δ2.38(s,6H,-CH 3 ), 4.09 (br, 1H, -NH), 6.46-6.62 (m, 3H, Ar), 6.92-7.21 (m, 8H, Ar), 7.87 (d, J=7.8Hz, 1H, Ar), 8.19 ( d, J=7.8 Hz, 1H, Ar), 8.50 (s, 1H, -N=CH).
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