Pd complex catalyst, preparation method and application thereof
A catalyst and complex technology, applied in the field of chemistry, can solve the problems of difficult separation of palladium catalyst, difficult recovery and reuse of palladium black, etc., and achieve the effects of good stability, catalysis and high catalytic activity.
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Embodiment 1
[0032] 2,6-bis(methyl)aniline (2.3mmol) and 2-(2,6-bis(benzhydryl)-4-chlorophenylimine)acenaphthylen-1-one (1.44g, 2.3mmol) Add 150 mg of p-toluenesulfonic acid as a catalyst, reflux and stir in 100 mL of toluene for 6 h, remove the solvent after filtration, dissolve the residue in dichloromethane, pass through a silica gel column, and rinse with petroleum ether / ethyl acetate (50:1). The two streams were divided into products, and the solvent was removed to obtain a yellow solid, which was Ligand 1.
[0033] Preparation of Pd complex catalyst 1 (R is methyl): under the protection of N2, PdCl 2 (CH 3 EN) 2 (0.04g, 0.14mmol) and ligand 1 (0.11g, 0.14mmol) were added to 10mL of dichloromethane, stirred at room temperature for 12h, passed through a silica gel column, and washed out with petroleum ether / ethyl acetate (5:1) One fraction and the second fraction were rinsed with dichloromethane, and the second fraction was collected to obtain a Pd complex catalyst. The solvent was ...
Embodiment 2
[0035] 2,6-bis(ethyl)aniline (2.3mmol) and 2-(2,6-bis(benzhydryl)-4-chlorophenylimine)acenaphthylen-1-one (1.44g, 2.3mmol) Add 150 mg of p-toluenesulfonic acid as a catalyst, reflux and stir in 100 mL of toluene for 6 h, remove the solvent after filtration, dissolve the residue in dichloromethane, pass through a silica gel column, and rinse with petroleum ether / ethyl acetate (50:1). The two streams were divided into products, and the solvent was removed to obtain a yellow solid, which was Ligand 2.
[0036] The preparation of Pd complex catalyst 2 (R is ethyl) was the same as in Example 1, except that the ligand was ligand 2, and 82 mg of red solid was obtained with a yield of 62.7%. IR(KBr):3061,2966,2927,2875,1622,1600,1576,1494,1445,1299,1178,1099,765,741,700cm -1 . 1 H NMR (400MHz, CDCl 3 ,TMS):δ=7.87(d,J=8.20Hz,1H),7.66(d,J=8.27Hz,1H),7.49(t,J=7.82Hz,1H),7.36–7.22(m,13H) ,7.13(d,J=7.60Hz,4H),7.04(s,2H),6.98(t,J=7.44Hz,1H),6.47(t,J=7.48Hz,6H),6.38(d,J= 7.24Hz,1H),6.19...
Embodiment 3
[0038] 2,6-bis(methyl)aniline (2.3mmol) and 2-(2,6-bis(benzhydryl)-4-chlorophenylimine)acenaphthylen-1-one (1.44g, 2.3mmol) Add 150 mg of p-toluenesulfonic acid as a catalyst, reflux and stir in 100 mL of toluene for 6 h, remove the solvent after filtration, dissolve the residue in dichloromethane, pass through a silica gel column, and rinse with petroleum ether / ethyl acetate (50:1). The two streams were divided into products, and the solvent was removed to obtain a yellow solid, which was Ligand 3.
[0039] Pd complex catalyst 3 (R 1 propyl) was the same as in Example 2, except that the ligand was ligand 3, and 80 mg of a red solid was obtained with a yield of 59.9%. IR(KBr):3060,2964,2870,1622,1600,1577,1494,1442,1300,1181,1079,768,744,700cm -1 . 1 H NMR (400MHz, CDCl 3 ,TMS):δ=7.87(d,J=8.30Hz,1H),7.63(d,J=8.38Hz,1H),7.54(t,J=7.81Hz,1H),7.37(m,7H),7.30 -7.22(m,6H),7.09(d,J=7.59Hz,4H),7.04(s,2H),6.93(t,J=7.83Hz,2H),6.48(t,J=7.43Hz,4H) ,6.42(s,2H),6.34(d,J=7.26Hz,1H),6.2...
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