Method for preparing transition metal complexes, transition metal complexes prepared using the metod, catalyst composition containing the complexes
a technology catalyst compositions, which is applied in the field of preparation of transition metal complexes, transition metal complexes prepared using the method, and catalyst compositions containing transition metal complexes, can solve the problems of copolymerization performance and compound activity not showing enhanced activity, and achieve high yield, large steric hindrance, and the effect of transition metal complex
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example 1
Preparation of 8-(2,3,4,5-tetramethyl-1,3-cyclopentadienyl)-1,2,3,4-tetrahydroquinoline (Compound 3a)
[0130]1,2,3,4-tetrahydroquinoline (13.08 g, 98.24 mmol) and diethylether (150 mL) were put into a Schlenk flask. The Schlenk flask was immersed in a dry ice / acetone cooling bath at −78° C., and shaken for 30 minutes. Then, n-BuLi (n-butyl lithium, 39.3 mL, 2.5 M, 98.24 mmol) was introduced thereto using a syringe under nitrogen atmosphere to form a pale yellow slurry. Thereafter, the flask was shaken for 2 hours, and then the flask was warmed to ambient temperature while removing the resulting butane gas. The flask was again immersing into the cooling bath at −78° C., and then a CO2 gas was introduced thereto. As introducing carbon dioxide gas, the slurry gradually disappeared to form a clear solution. The flask was connected into a bubbler to remove the carbon dioxide gas, while raising the temperature to ambient temperature. Thereafter, excess CO2 gas and the solvent were removed u...
example 2
Preparation of [(1,2,3,4-tetrahydroquinolin-8-yl)tetramethylcyclopentadienyl-eta5,kapa-N]titanium dimethyl (Compound 5a)
[0134]In a dry box, the compound 3a (8.07 g, 32.0 mmol) as prepared in Example 1 and diethylether (140 mL) were put into a round flask, and cooled to −30° C. n-BuLi (17.7 g, 2.5 M, 64.0 mmol) was slowly added thereto under stirring. While raising the temperature to ambient temperature, reaction was performed for 6 hours. Thereafter, the mixture was washed with diethylether several times, and filtered to obtain a solid. The remaining solvent was removed under vacuum to obtain a dilithium compound (Compound 4a) (9.83 g) as a yellow solid. The yield was 95%.
[0135]1H NMR (C6D6, C5D5N): δ 2.38 (br s, 2H, quin-CH2), 2.53 (br s, 12H, Cp-CH3), 3.48 (br s, 2H, quin-CH2), 4.19 (br s, 2H, quin-CH2), 6.77 (t, J=6.8 Hz, 2H, quin-CH), 7.28 (br s, 1H, quin-CH), 7.75 (br s, 1H, quin-CH) ppm.
[0136]In a dry box, TiCl4.DME (4.41 g, 15.76 mmol) and diethylether (150 mL) were put into...
example 3
Preparation of 5-indenyl-1,2,3,4-tetrahydroquinoline (Compound 3b)
[0138]The procedure was carried out in the same manner as the preparation method of [Example 1] except that indenone was used instead of tetramethylcyclopentanone, and the resultant was purified by column chromatography using a hexane:ethyl acetate (v / v, 20:1) solvent to obtain a yellow oil. The yield was 49%.
[0139]1H NMR (C6D6): δ 1.58-1.64 (m, 2H, quin-CH2), 2.63 (t, J=6.8 Hz, 2H, quin-CH2), 2.72-2.77 (m, 2H, quin-CH2), 3.17 (d, J=2.4 Hz, 2H, indenyl-CH2), 3.85 (br s, 1H, N—H), 6.35 (t, J=2.0 Hz, 1H, indenyl-CH), 6.76 (t, J=7.6 Hz, 1H, quin-CH), 6.98 (d, J=7.2 Hz, 1H, quin-CH), 7.17 (td, J=1.6, 7.2 Hz, 1H, quin-CH), 7.20 (td, J=1.6, 7.2 Hz, 2H, indenyl-CH), 7.34 (d, J=7.2 Hz, 1H, indenyl-CH), 7.45 (dd, J=1.2, 6.8 Hz, 1H, indenyl-CH) ppm. 13C NMR (C6D6): δ 12.12, 23.08, 27.30, 48.84, 51.01, 119.70, 119.96, 120.95, 126.99, 128.73, 131.67, 136.21 ppm.
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