A bridged metallocene compound catalyst, its preparation method and its application
A metallocene compound and catalyst technology, applied in metallocene, chemical instruments and methods, organic chemistry, etc., can solve the problems of fast chain transfer, small steric hindrance of substituent groups, and insufficient rigidity, and achieve good mechanical properties and processing performance, good catalytic activity, wide application prospects
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Embodiment 1
[0039] (1) Synthesis of compound a
[0040] Add 0.25mol 3,5-dichlorobenzonitrile and 100mL dry diethyl ether to a 500mL three-neck flask, then add 3.5g metallic lithium at -20°C and react for 20 hours, then add 0.5mol monomethyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 100 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 50 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 22.73 g of white solid, yield 46%.
[0041] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.48 mol cyclopentadiene sodium dropwise at -30 ° C for 12 hours, remove the solvent in vacuo, and extract the residual solid with 50 mL of ether three times, and then place it in an ice-water bath Slowly add 192mL of 2.5M n-butyllithium hexane solution dropwise, then stir at ...
Embodiment 2
[0047] (1) Synthesis of compound b
[0048] Add 0.12mol 3,5-dichlorobenzonitrile and 80mL dry diethyl ether to a 500mL three-neck flask, then add 1.7g metallic lithium at -20°C and react for 20 hours, then add 0.25mol monomethyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 80 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 30 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 11.53 g of white solid, yield 46%.
[0049] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.24 mol of indenyllithium dropwise at -30°C for 12 hours, remove the solvent in vacuo, extract the residual solid with 50 mL of ether three times, and then slowly drop it in an ice-water bath Add 81mL of 2.5M n-butyllithium hexane solution, then stir at room temperature for 12...
Embodiment 3
[0055] (1) Synthesis of compound c
[0056] Add 0.06mol 3,5-dichlorobenzonitrile and 60mL dry diethyl ether to a 500mL three-necked flask, then add 0.84g metallic lithium at -20°C and react for 20 hours, then add 0.12mol phenyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 60 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 30 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 12.15 g of white solid, yield 44%.
[0057] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.12 mol of sodium cyclocene at -30°C and react for 12 hours, remove the solvent in vacuo, extract the residual solid with 50 ethyl ether three times, and then slowly add 40mL of 2.5M n-butyllithium hexane solution, then stirred at room temperature for 12 hours, filtered, and va...
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