A bridged dinuclear metallocene compound for SPP and its preparation method and application
A technology of metallocene compounds and compounds, applied in metallocenes, chemical instruments and methods, organic chemistry, etc., can solve the problem of molecular weight reduction, etc., and achieve the effect of simple steps, high syndiotacticity, and less co-catalysts
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Embodiment 1
[0057] Ligand L1[(C 5 h 4 )CH(( t Bu) 2 C 13 h 9 )] 2 (CH 2 ) 4 Synthesis
[0058] Ligand L1[(C 5 h 4 )CH(( t Bu) 2 C 13 h 9 )] 2 (CH 2 ) 4 The synthetic route of is as follows:
[0059]
[0060] Under ice-bath, cyclopentadiene (75mL, 911.5mmol) was added dropwise to adipaldehyde (51.95g, 455.7mmol), in methanol solution, and pyrrolidine 45mL was slowly added dropwise under ice-water bath, gradually turning yellow, and yellow slowly Deepen slowly, react for 5 hours, add water, adjust the pH to neutral with acetic acid, separate the liquids, take the organic phase, extract the water phase with anhydrous ether for 3 times, combine the organic phases, wash with saturated NaCl, anhydrous MgSO 4 Dry; filter, spin off the solvent, use petroleum ether as the mobile phase, separate by column chromatography, collect the second fraction, and concentrate to obtain 33.49 g of difulvene, with a yield of 35%.
[0061] Under ice bath, bridged bisfulvene (6.3g, 30mmol) w...
Embodiment 2
[0067] Ligand L2[(C 5 h 4 )CH(C 13 h 9 )] 2 (CH 2 ) 2 Synthesis
[0068] Same as Example 1, succinic dialdehyde replaces adipaldehyde to prepare bridged fulvene;
[0069] Under ice bath, bridged bisfulvene (6.3g, 30mmol) was added dropwise to a solution of lithium fluorene (9.96g, 60mmol) in ether (150mL), a precipitate formed, refluxed for two days, hydrolyzed, acetic acid adjusted the pH to neutral , liquid separation, take the organic phase, extract the aqueous phase with ether twice, combine the organic phases, wash with saturated brine, dry over anhydrous magnesium sulfate for 6 h, filter, spin off the solvent in vacuo, use petroleum ether as the mobile phase, and separate by column chromatography, After concentration, 4.59 g of L2 was obtained, yield 30%.
[0070] Complex 2[(C 5 h 4 )CH(C 13 h 8 )ZrCl 2 ] 2 (CH 2 ) 2 Synthesis
[0071] Under ice-water bath conditions, n BuLi (8mmol) was added dropwise to the ether solution of the ligand (1.02g, 2mmol), ...
Embodiment 3
[0075] Ligand L3[(C 5 h 4 )CH(C 13 h 9 )] 2 (CH 2 ) 3 synthesis of synthesis
[0076] Same as Example 1, glutaraldehyde replaces adipaldehyde to prepare bridged fulvenes;
[0077] Under ice bath, bridged bisfulvene (5.88g, 30mmol) was added dropwise to a solution of lithium fluorene (9.96g, 60mmol) in ether (250mL), a little precipitate formed, and after one day of reaction, there was still a small amount of precipitate, hydrolysis, acetic acid Adjust the pH to neutral, separate the liquids, take the organic phase, extract the aqueous phase with ether twice, combine the organic phases, wash with saturated brine, dry with anhydrous magnesium sulfate for 6 hours, filter, and spin off the solvent in vacuo, using petroleum ether as the mobile phase, After separation by column chromatography and concentration, 5.82 g of L3 was obtained with a yield of 37%.
[0078] Complex 3[(C 5 h 4 )CH(C 13 h 8 )ZrCl 2 ] 2 (CH 2 ) 3 Synthesis
[0079] Under ice-water bath conditi...
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