Beta-ketoimine rare earth metal catalyst, preparation method and application
A β-ketimine rare earth and metal catalyst technology, which is applied in chemical instruments and methods, organic chemistry, compounds containing periodic table Group 3/13 elements, etc., can solve the problem that the application of β-ketimine rare earth metal catalysts has not been Some people reported and other problems, to achieve the effect of simple operation, good environmental protection and high economic efficiency
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Embodiment 1
[0060] (1) Preparation of β-ketimine ligand
[0061]
[0062] First, in the glove box, 4.0g (27.74mmol) of 8-aminoquinoline and 5.56g (55.53mmol) of 2,4-pentanedione were added to the eggplant bottle respectively, and dissolved with 50ml of toluene to obtain the mixture a. Take the eggplant bottle out of the glove box, put it into an oil bath, reflux, and add 7d formic acid dropwise to mixture a under stirring to obtain mixture b;
[0063] Next, the reactor containing the mixture b was heated to 110° C. under a nitrogen atmosphere, and after 48 hours of reaction, the eggplant bottle was taken out and cooled to 25° C. to obtain the mixture c.
[0064] Finally, add saturated brine to the mixture c, extract, separate layers to obtain an aqueous phase and an organic phase, and add anhydrous MgSO to the organic phase 4 After 10g, filter, take liquid and carry out vacuum distillation to obtain solid powder, adopt the method for column chromatography to obtain β-ketimine ligand,...
Embodiment 2
[0073] (1) Preparation of β-ketimine ligand
[0074]
[0075] First, in the glove box, 4.0g (27.74mmol) of 8-aminoquinoline and 5.56g (55.53mmol) of 2,4-pentanedione were added to the eggplant bottle respectively, and dissolved with 50ml of toluene to obtain the mixture a. Take the eggplant bottle out of the glove box, put it into an oil bath, reflux, and add 7d formic acid dropwise to mixture a under stirring to obtain mixture b;
[0076] Next, the reactor containing the mixture b was heated to 115° C. under a nitrogen atmosphere, and after 46 hours of reaction, the eggplant bottle was taken out and cooled to 25° C. to obtain the mixture c.
[0077] Finally, add saturated brine to the mixture c, extract, separate layers to obtain an aqueous phase and an organic phase, and add anhydrous MgSO to the organic phase 4 After 10g, filter, take liquid and carry out vacuum distillation to obtain solid powder, adopt the method for column chromatography to obtain β-ketimine ligand, be...
Embodiment 3
[0086] Put the reactor in the glove box, add 10 μmol β-ketimine scandium catalyst, 5 mL o-dichlorobenzene, 20 μmol Al i Bu 3 , 8mmol isoprene and 10μmol[Ph 3 C][B(C 6 f 5 ) 4 ], after stirring and reacting at ‐30°C for 24 hours, the eggplant bottle was taken out, and 30 mL of ethanol containing 5% 2,6-di-tert-butyl-4-methylphenol was added to terminate the reaction; the reaction solution was settled with ethanol, A white viscous solid substance was precipitated, and the solid substance was vacuum-dried at 45° C., and the solvent was removed to a constant weight to obtain polyisoprene with a net weight of 0.545 g, a conversion rate of 100%, and a polymerization activity of 2.27 kg·mol -1 h -1 , cis-1,4-polymerization selectivity 99.5%.
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