Rare earth complex, catalyst composition for preparation of isoprene rubber and preparation method thereof, and preparation method of isoprene rubber
A rare earth complex, rare earth technology, applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, compounds containing elements of Group 3/13 of the periodic table, etc. Problems such as wide molecular weight distribution
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preparation example 1
[0079] Preparation of benzyl-3-(2,6-diisopropylphenylimino)indole:
[0080] Dissolve 1-benzyl-3-indolecarbaldehyde (2.35g, 10mmoL) in 20mL of absolute ethanol, add 2,6-diisopropylaniline (1.77g, 10mmoL) dropwise, and add 0.5 mmoL of p-toluenesulfonic acid was reacted at 25° C. for 12 h, and the obtained solid powder was washed with absolute ethanol and dried, weighing 2.64 g, and the yield was 67%.
[0081] Characterization data are:- 1 H NMR (300MHz, CDCl 3 ,ppm):1.15(d,J=6.6Hz,12H,CHMe 2 ),3.08(m,2H,CHMe 2 ),5.34(s,2H,CH 2 C 6 h 5 ), 7.05-7.33 (m, 11H), 7.50 (s, 1H, 2-indole), 8.29 (s, 1H, CH=N), 8.51 (d, J=3.6Hz, 1H, 4-indole); 13 C NMR (75MHz, CDCl 3 ,ppm):23.60,27.93,50.61,110.06,115.34,121.73,122.73,122.89,123.43,123.48,126.34,127.16,128.09,129.00,133.37,136.36,137.51,310.5; 1 H NMR (300MHz,C 6 D. 6 ,ppm): 1.43(d,J=9Hz,12H,CHMe 2 ), 3.61 (m, J=6Hz, 2H, CHMe 2 ),4.71(s,2H,CH 2 C 6 h 5 ),6.87-6.89(m,2H),6.93(s,1H,2-indole),7.11-7.13(m,3H),7.28-7.46(m,6H),8....
preparation example 2
[0083] Preparation of methyl-3-(2,6-diisopropylphenylimino)indole:
[0084] Dissolve 1-methyl-3-indole formaldehyde (1.59g, 10mmoL) in 20mL of absolute ethanol, add 2,6-diisopropylaniline (1.77g, 10mmoL) dropwise, and add 0.5 mmoL of p-toluenesulfonic acid was reacted at 25°C for 12h, and the obtained solid powder was washed with absolute ethanol and dried, weighing 1.72g, and the yield was 54%.
[0085] The characterization data is: 1 H NMR (300MHz, CDCl3, ppm): 1.20(d, J=6.9Hz, 12H), 3.15(m, 2H), 3.88(s, 3H), 7.07-7.42(m, 6H), 7.50(s, 1H ),8.34(s,1H),8.51(d,J=7.5Hz,1H); 13 C NMR (75MHz, CDCl 3 ,ppm):23.56,27.96,33.25,109.52,114.73,121.55,122.51,122.89,123.31,123.40,133.96,137.90,138.16,155.59; 1H NMR(300MHz,C6D6,ppm):9.05(Hz,d, 1H, 4-indole), 8.39(s, 1H, CH=N), 7.25-7.37(m, 5H), 7.02(d, J=9Hz, 1H), 6.62(s, 1H, 2-indole), 3.54 (m, J=6Hz, 2H, CHMe2), 2.88 (s, 3H, N-CH3), 1.38 (d, J=6Hz, 12H, CHMe2). 13 C NMR (75MHz, C6D6, ppm): 23.59, 28.34, 31.92, 109.33, 115.08, 121.84...
Embodiment 1
[0087] The preparation of the rare earth complex of structure shown in formula (A1):
[0088]
[0089] To contain Y(CH 2 SiMe 3 ) 3 (THF) 2 (0.26g, 0.52mmoL) in 15mL of n-hexane solution was slowly added dropwise the toluene containing 1-benzyl-3-(2,6-diisopropylphenylimino) indole (0.334g, 1.04mmoL) The solution was 5 mL, reacted at 25°C for 4 hours, the solvent was removed under reduced pressure, and the remaining solid was extracted twice with n-hexane, each time with 8 mL of n-hexane, the obtained n-hexane solution was concentrated to 10 mL, and the concentrated solution was left standing at 0°C to obtain yellow crystals 0.32 g, 64% yield.
[0090] Elemental analysis results (%): Calculated value (C 60 h 69 N 4 SiY): C, 74.82; H, 7.22; N, 5.82. Measured value: C, 74.56; H, 7.54; N, 5.58. 1 H NMR (300MHz, C 6 D. 6 ,ppm):0.08(s,9H,SiMe 3 ),0.26(d,J=21.00,2H,CH 2 SiMe 3 ), 0.51 (d, J=6.78, 6H, CHMe 2 ), 1.13 (d, J=6.81, 6H, CHMe 2), 1.36 (d, J=5.49, 6H, CHMe...
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