Triazole-copper trifluoromethanesulfonate complex with catalytic 4-tert-butylphenylboronic acid and preparation method thereof
A technology of tert-butylbenzeneboronic acid and benzenebistriazole copper, which is applied to copper organic compounds, organic compounds/hydrides/coordination complex catalysts, hydrocarbons, etc., can solve the problems such as expensive palladium catalysts, and achieve the reaction The operation is simple and easy, the reaction yield is high, and the production cost is low.
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Embodiment 1
[0028] Preparation of 4-(3-(4H-1,2,4-triazol-4-yl)phenyl)-4H-1,2,4-triazole (L) Ligand
[0029] Add m-phenylenediamine (1mmol) and bisformylhydrazide (2mmol) respectively into a 50mL three-necked round-bottomed flask equipped with a magnet, reflux condenser, and thermometer, start stirring at 100°C, and react for 12 hours. After the reaction was completed, the reaction solution was cooled to room temperature, and a large amount of precipitate was precipitated, which was recrystallized with water and ethanol, and the yield was 86%. Elemental Analysis C 10 h 8 N 6 Theoretical: C, 56.60; H, 3.80; N, 39.60. Experimental values: C, 56.56; H, 3.75; N, 39.56. The molar ratio of m-phenylenediamine to bisformylhydrazide is 1:2.
Embodiment 2
[0031] Cu(CF 3 SO 3 ) 2 The molar ratio of 4-(3-(4H-1,2,4-triazol-4-yl)phenyl)-4H-1,2,4-triazole)(L) is 1:1;
[0032] L (0.0424g, 0.2mmol), Cu(CF 3 SO 3 ) 2 (0.0691g, 0.2mmol), H 2 O (6mL), CH 3 CN (4mL), water heat 100 oAfter three days in C, it was slowly lowered to room temperature. After opening the kettle, there are yellow rod-shaped crystals suitable for X-ray single crystal diffraction analysis. Yield: 35% (calculated based on L). Elemental analysis (C 33 h 26 Cu 3 f 9 N 18 o 10 S 3 ) Theoretical value (%): C, 30.67; H, 2.03; N, 19.51. Found: C, 30.69; H, 2.06; N, 19.59.
[0033] We also tried other ratios such as Cu(CF 3 SO 3 ) 2 If the molar ratio to L is 2:1, no crystalline compound can be obtained no matter how long the hydrothermal reaction time is. Therefore Cu(CF 3 SO 3 ) 2 The molar ratio of L and L is 1:1 is the best reaction ratio.
Embodiment 3
[0035] The crystal structure was determined by APEXIICCD single crystal diffractometer, using graphite monochromatized Mokα ray (λ=0.71073?) as the incident radiation, collecting diffraction points by ω-2θ scanning, and correcting the unit cell parameters by the least square method. The difference Fourier electron density map was solved for the crystal structure using software and corrected for Lorentz and polarization effects. All H atoms were synthesized by difference Fourier transform and determined by ideal position calculation. The detailed crystal determination data are shown in Table 1. Structural primitives see figure 1 , the three-dimensional structure of the complex see figure 2 .
[0036] Table 1. Crystallographic data of complex 1
[0037]
[0038]
PUM
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