Metallocene compound
a technology of metalocene compound and compound, which is applied in the field of metalocene compound, to achieve the effects of excellent activity, long residence time, and high molecular weigh
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preparation example 1
n-2-yl)methyl)trimethylsilane
[0107]
[0108]3.7 ml (30 mmol) of 2-Bromo-1H-indene was added to a flask, and Ar bubbling was performed for about 5 minutes while stirring in the presence of 100 ml of THF to remove dissolved gas. Under Ar bubbling, 0.8 g (1.5 mmol) of Ni(dppe)Cl2 was rapidly added and 30 ml (30 mmol) of 1.0 M ((Trimethylsilyl)methyl)magnesium chloride dissolved in diethyl ether at room temperature was slowly added dropwise. And then, the reaction was continued overnight while refluxing under Ar condition at 80° C. (dppe=1,2-Bis(diphenylphosphino)ethane)
[0109]50 mL of water was added thereto, and the organic layer was extracted three times with 50 mL of diethylether. An appropriate amount of MgSO4 was added to the collected organic layer, stirred for a while, filtered, and the solvent was dried under reduced pressure.
[0110]The resulting product was confirmed by 1H-NMR.
[0111]1H-NMR (500 MHz, CDCl3): 0.03 (9H, s), 3.25 (2H, s), 6.3 (1H, s), 7.02-7.32 (4H, m)
example 1-1
f Ligand Compound
[0112]
[0113]After dissolving 1.01 g (5 mmol) of ((1H-inden-3-yl)methyl)trimethylsilane in 80 ml of Hexane and 2.4 ml of MTBE, 2.4 mL (6 mmol) of a 2.50 M n-BuLi hexane solution was added thereto dropwise in a dry ice / acetone bath. The reaction mixture was slowly warmed up to room temperature, and then stirred for 24 hours, followed by addition of 50 ml of Hexane.
[0114]Another 250 mL Schlenk flask was placed in the glove box and weighed 1.36 g (5 mmol) of SiCH3Cl2(CH2)6(t-BuO) in the glove box. Then, it was taken out of the glove box, dissolved in 50 mL of Hexane, and then the mixture prepared above was added thereto dropwise in a dry ice / acetone bath (Synthesized Compound 1-1).
[0115]Separately, after dissolving 1.01 g (5 mmol) of ((1H-inden-2-yl)methyl)trimethylsilane of the Preparation Example 1 in 50 ml of THF, 2.4 mL (6 mmol) of a 2.50 M n-BuLi Hexane solution was added thereto dropwise in a dry ice / acetone bath. The reaction mixture was slowly warmed up to room ...
example 1-2
f Metallocene Compound
[0120]
[0121]After dissolving 3.02 g (4.7 mmol) of the ligand compound synthesized in Example 1-1 in 80 mL of toluene and 2.6 mL of MTBE in a 250 mL Schlenk flask which is dried in an oven, 4.4 mL (11 mmol) of a 2.5 M n-BuLi Hexane solution was added thereto dropwise in a dry ice / acetone bath. The reaction mixture was slowly warmed up to room temperature, and then stirred for 24 hours, followed by lithiation.
[0122]1.88 g (5 mmol) of ZrCl4(THF)2 was taken in a glove box and injected into another 250 mL Schlenk flask to prepare a suspension having 80 mL of toluene. The above two flasks were cooled down to −78° C. and the lithiated ligand compound was slowly added to the toluene suspension of ZrCl4(THF)2. After the completion of the injection, the reaction mixture was slowly warmed up to room temperature, stirred for one day and subjected to reaction. Then, toluene in the mixture was removed up to a volume of about ⅕ through vacuum-reduced pressure. Hexane was adde...
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