Iron-based complex, preparation method thereof and method for preparing polycyclohexene oxide under catalysis of iron-based complex
A technology for epoxycyclohexane and complexes, which is applied in the field of iron-based complexes and their preparation, can solve the problems of expensive palladium chloride, high reaction temperature, complicated operation process, etc., and achieve good industrial application prospects and reaction conditions Mild, simple preparation conditions
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Example Embodiment
[0054] Example 1
[0055] The present embodiment provides an iron-based complex, which is prepared by the following steps:
[0056] (1) Synthesis of Ligand-1: Under an argon atmosphere, a tetrahydrofuran (20mL) solution dissolved in 2-hydroxy-aniline (0.54g, 5mmol) was added to a tetrahydrofuran (20mL) solution dissolved in 2,4-dichloro-6-chloromethylphenol (2.56g, 10mmol) in a 100 mL reaction bottle, and then triethylamine (1.4mL, 10.07mmM) was added to the reaction bottle. The reaction is stopped after 10h of heating reflux, and the white precipitate is removed by filtration after cooling. Rotational evaporation removes the solvent to give a reddish-brown oily substance. By column chromatography (petroleum ether: ethyl acetate = 5:2), a white solid (1.6g, 70%), which was obtained 1 See H NMR spectra Figure 1A , 13 See C NMR spectra Figure 1B , its ultraviolet spectra are seen Figure 5 ; 1 H NMR(500MHz,CDCl 3 )δ7.21(d,J=2.5Hz,2H),7.15(dd,J=7.9,1.3Hz,1H),7.05(td,J=8.0,1.4Hz,1H),7.00
Example Embodiment
[0058] Example 2
[0059] The present embodiment provides an iron-based complex, which is prepared by the following steps:
[0060] (1) Ligand-2: In an argon atmosphere, the tetrahydrofuran (20mL) solution dissolved in 2-hydroxy-5-chloro-aniline (0.72g, 5mmol) was added to the tetrahydrofuran (20mL) solution dissolved in 2,4-dichloro-6-chloromethylphenol (2.56g, 10mmol) in a 100mL reaction bottle, and then triethylamine (1.4mL, 10.07mmol) was added to the reaction bottle. The reaction is stopped after 10h of heating reflux, and the white precipitate is removed by filtration after cooling. Rotational evaporation removes the solvent to give a reddish-brown oily substance. By column chromatography (petroleum ether: ethyl acetate = 2:1), a white solid (1.9g, 77%), which is obtained 1 See H NMR spectra Figure 2A , 13 See C NMR spectra Figure 2B , its ultraviolet spectra are seen Figure 5 。 1 H NMR(500MHz,CDCl 3 )δ7.22(d,J=2.3Hz,2H),7.15(d,J=2.2Hz,1H),7.02(dd,J=10.6,2.2Hz,3H),6.86(d,J=8.6H
Example Embodiment
[0062] Example 3
[0063] The present embodiment provides an iron-based complex, which is prepared by the following steps:
[0064] (1) Ligand-3: In an argon atmosphere, a tetrahydrofuran (20mL) solution dissolved in 2-hydroxy-5-methyl-aniline (0.61g, 5mmol) was added to a tetrahydrofuran (20mL) solution dissolved in a 100 mL reaction bottle, and then triethylamine (1.4mL, 10.07mmol) was added to the reaction bottle. The reaction is stopped after 10h of heating reflux, and the white precipitate is removed by filtration after cooling. Rotational evaporation removes the solvent to give a reddish-brown oily substance. By column chromatography (petroleum ether: ethyl acetate = 2:1), a white solid (1.7g, 72%), thereof 1 See H NMR spectra Figure 3A , 13 See C NMR spectra Figure 3B , its ultraviolet spectra are seen Figure 5 。 1 H NMR(500MHz,CDCl 3)δ7.20(d,J=2.3Hz,2H),7.02–6.92(m,3H),6.83(dd,J=18.0,8.1Hz,2H),4.11(s,4H),2.25(s,3H); 13 C NMR(126MHz,CDCl 3 )δ149.61(s),149.13(s),134.84(s),129.
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