A kind of enol type zinc compound, its preparation method and its application as catalyst
A zinc compound, enol technology, applied in the field of polymers, can solve the problems of low catalytic reaction activity, difficult to meet actual needs and other problems
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[0048] The present invention also provides a kind of preparation method of enol zinc compound, comprising the following steps:
[0049] The enol formula ligand having the structure shown in formula (II) is reacted with the organozinc compound in a solvent to obtain the enol formula zinc compound having the structure shown in formula (I); the organozinc compound is a silazane group Zinc;
[0050]
[0051] Among them, Y is -CH 2 -CH 2 -or-CH 2 -CH2 -CH 2 -;
[0052] R is one of alkyl, haloalkyl and phenyl.
[0053] Specifically, the R is preferably one of an alkyl group with 1 to 5 carbon atoms, a halogenated alkyl group with 1 to 5 carbon atoms, and a phenyl group; more preferably -CH 3 、-CF 3 and one of phenyl.
[0054] In the present invention, the enol type zinc compound having the structure represented by the formula (I) is obtained by reacting the enol type ligand having the structure represented by the formula (II) and the organozinc compound as raw materials. ...
Embodiment 1
[0087] Dissolve 1.80g of N,N-dimethylethylenediamine in 20mL of ethanol to obtain N,N-dimethylethylenediamine solution; dissolve 2.00g of acetylacetone in 30mL of ethanol to obtain an acetylacetone solution. The solution was slowly added dropwise to the N,N-dimethylethylenediamine solution, and the resulting mixed solution was refluxed at 78° C. for 14 hours to obtain a reaction mixture. The solvent in the reaction mixture was removed by rotary evaporation, and the obtained reaction product was purified by column chromatography. The eluent of the column chromatography was a mixed solution of n-hexane and ethyl acetate to obtain the enol ligand.
[0088] The present invention carries out nuclear magnetic resonance analysis to the enol formula ligand that obtains, and the result is as follows:
[0089] 1 H NMR (300MHz, CDCl 3 ): δ=10.74(s OH 1H), 4.86(s CHCOH1H), 3.20(q C=NCH 2 2H), 2.37 (t C = NCH 2 CH 2 N(CH 3 ) 2 2H), 2.16(s(CH 3 ) 2 N 6H), 1.88 (s CH 3 C=N 3H), 1....
Embodiment 2
[0091] Dissolve 1.80g of N,N-dimethylethylenediamine in 20mL of ethanol to obtain N,N-dimethylethylenediamine solution; dissolve 3.30g of 1-phenyl-1,3-butanedione in 30mL of ethanol , to obtain 1-phenyl-1,3-butanedione solution, slowly add 1-phenyl-1,3-butanedione solution to N,N-dimethylethylenediamine solution, and the obtained mixed solution Reflux at 78°C for 12h to obtain a reaction mixture. The solvent in the reaction mixture was removed by rotary evaporation, and the obtained reaction product was purified by column chromatography. The eluent of the column chromatography was a mixed solution of n-hexane and ethyl acetate to obtain the enol ligand.
[0092] The present invention carries out nuclear magnetic resonance analysis to the enol formula ligand that obtains, and the result is as follows:
[0093] 1 H NMR (400M, CDCl 3 ): δ=8.14(d,2H,ArH), 7.45(d,3H,ArH), 5.71(s,1H,CHCOH), 3.49(q,2H,C=NCH 2 ), 2.62(t,2H,C=NCH 2 CH 2 N(CH 3 ) 2 ), 2.34(s,6H,(CH 3 ) 2 N), 2...
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