Alpha diimine palladium compound catalyst containing ferrocene group, preparation method and application thereof
A technology based on α-diimine palladium and ferrocenyl, which is applied in the field of preparation of α-diimine palladium catalysts and their ligands, and can solve problems such as vacancy and no one has achieved redox regulation
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[0075] The following examples illustrate the specific content of the present invention. The data provided include the synthesis of ligands, the synthesis of metal compounds, ethylene polymerization or copolymerization methods, wherein the synthesis of complexes and the polymerization process are carried out under anhydrous and oxygen-free conditions. Yes, all sensitive substances are stored in a glove box, all solvents are strictly dried to remove water, ethylene gas is purified by water and oxygen removal columns, and methyl acrylate is purified by water and oxygen removal under reduced pressure distillation. Without special instructions, all raw materials are used directly after purchase.
[0076] Silica gel column separation adopts 200-300 mesh silica gel. NMR detection adopts Bruker 400MHz NMR instrument. Elemental analysis was determined by the Physics and Chemistry Center of University of Science and Technology of China. Weight average molecular weight and molecular we...
preparation example 1
[0088] Preparation Example 1: Synthesis of 2,3-bis(2,6-diisopropyl-4-ferrocenylaniline)-butane
[0089]
[0090] Add 0.5 g of 2,6-diisopropyl-4-ferrocenylaniline, 0.06 g of 2,3-butanedione, 20 ml of toluene and a catalytic amount of p-toluenesulfonic acid in a 50 ml round bottom flask at room temperature . After raising the temperature to 80° C. for 12 hours, the temperature was raised again to 120° C. and refluxed for 24 hours. Cool down to room temperature, add diethyl ether to extract, wash with brine three times, and dry over anhydrous magnesium sulfate. The solvent was drained and separated by column chromatography (silica gel phase, petroleum ether: ethyl acetate = 40:1) to obtain an orange-yellow product. The yield is 66%. The measurement results for this product are as follows:
[0091] 1 H NMR (CDCl 3 , 400MHz): δ7.29(s, 4H, ArH), 4.62(s, 4H, C 5 h 4 ), 4.28(s, 4H, C 5 h 4 ), 4.06(s, 10H, C 5 h 5 ), 2.74 (sept, J=6.8, 4H, CHMe 2 ), 2.11 (s, 6H, N=CMe),...
preparation example 2
[0092] Preparation Example 2: Synthesis of 2,3-bis(2,6-diisopropyl-4-ferrocenylaniline)-butane palladium complex 1 (abbreviated as: Pd-Cl)
[0093]
[0094] At room temperature, 772 mg of the diimine ligand (i.e., 2,3-bis(2,6 diisopropyl-4-ferrocenylaniline)-butane) obtained in Preparation Example 1 was mixed with 265 mg of Pd ( COD)MeCl was stirred in 20 mL of dichloromethane for 12 hours. During stirring, the solid gradually dissolved, and the color of the solution changed from orange to dark red. After the reaction, the reactant was drained and separated with a silica gel column of 200-300 mesh silica gel, wherein a 1:1 mixture of sherwood oil and dichloromethane was used as the mobile phase, and then pure dichloromethane was used for column separation again. An orange-red solid was obtained with a yield of 94%. figure 1 A schematic diagram of the single crystal structure of the palladium catalyst with a ferrocenediamine ligand prepared in Preparation Example 2 of the ...
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