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Triazole-copper perchlorate complex with p-fluorophenylboronic acid catalyzing effect and preparation method of triazole-copper perchlorate complex

A technology of copper complexes and m-benzenebistriazole copper, which is applied in the direction of copper organic compounds, organic compounds/hydrides/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of expensive palladium catalysts and achieve reaction The effect of simple operation, high purity and high reaction yield

Inactive Publication Date: 2015-04-08
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the palladium catalyst is relatively expensive. If the expensive palladium catalyst can be replaced by a cheap copper complex to realize the reaction process, it can not only save costs, but also is expected to be industrialized.

Method used

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  • Triazole-copper perchlorate complex with p-fluorophenylboronic acid catalyzing effect and preparation method of triazole-copper perchlorate complex
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  • Triazole-copper perchlorate complex with p-fluorophenylboronic acid catalyzing effect and preparation method of triazole-copper perchlorate complex

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Experimental program
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Effect test

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 (1 mmol) and bisformylhydrazide (2 mmol) respectively into a 50 mL three-neck round-bottom flask equipped with a magnet, reflux condenser and thermometer, and start stirring at 100 ° C 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 and bisformylhydrazide is 1:2.

Embodiment 2

[0031] Cu(ClO 4 ) 2 and 4-(3-(4H-1,2,4-triazol-4-yl)phenyl)-4H-1,2,4-triazole) (L) in a molar ratio of 1:1;

[0032] L (0.0424 g, 0.2 mmol), Cu(ClO 4 ) 2 (0.0691 g, 0.2 mmol), H 2O (6 mL), CH 3 CN (4 mL), water hot 100 o After 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 10 h 8.5 ClCuN 6 o 4.25 ) Theoretical value (%): C, 30.67; H, 2.03; N, 19.51. Found: C, 30.63; H, 2.06; N, 19.59. We also tried other ratios such as Cu(ClO 4 ) 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(ClO 4 ) 2 The molar ratio of L and L is 1:1 is the best reaction ratio.

Embodiment 3

[0034] The crystal structure was determined using an APEX II CCD single crystal diffractometer, using graphite monochromatized Mokα rays (λ = 0.71073 ?) as the incident radiation. ω -2 θ Diffraction points are collected by scanning, and the unit cell parameters are obtained by least square method correction. The crystal structure is solved by software from the difference Fourier electron density map, and corrected by 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 .

[0035] Table 1 Complexes 1 The crystallographic data of

[0036]

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Abstract

The invention discloses a preparation method of {[Cu(L)] (ClO4).0.25H2O} (1) (L=4-(3-(4H-1, 2, 4-triazole-4-yl)phenyl)-4H-1, 2, 4-triazole). The complex is prepared by using a hydrothermal method comprising the step of reacting Cu(ClO4)2 and L under a 100-DEG C hydrothermal condition. The invention further discloses application of a copper complex, namely {[Cu(L)] (ClO4).0.25H2O} (1) (L=4-(3-(4H-1, 2, 4-triazole-4-yl)phenyl)-4H-1, 2, 4-triazole) as a catalyst for coupled reaction of p-fluorophenylboronic acid.

Description

[0001] The present invention has been funded by the National Natural Science Foundation of China (21471113), the Tianjin Municipal Education Commission project (20140506), the Tianjin Normal University academic innovation promotion project for young and middle-aged teachers, and the Tianjin Higher Education Innovation Team Training Program (TD12-5038). technical field [0002] The invention belongs to the technical field of inorganic synthesis and relates to copper complex {[Cu(L)](ClO 4 )·0.25H 2 O} (1) (L=4-(3-(4H-1,2,4-triazol-4-yl)phenyl)-4H-1,2,4-triazole) preparation method and as The application of the catalyst in the coupling reaction of fluorophenylboronic acid. Background technique [0003] The study of highly selective synthesis catalyzed by transition metal complexes has been an active field. Reactions that are difficult to achieve with common synthetic means can sometimes be completed in one step using transition metal complexes under mild conditions. Therefo...

Claims

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Application Information

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IPC IPC(8): C07F1/08B01J31/22C07C25/18C07C17/26
CPCB01J31/1815B01J2231/4277B01J2531/0213B01J2531/16C07C17/26C07C2531/22C07F1/08C07C25/18
Inventor 王英
Owner TIANJIN NORMAL UNIVERSITY
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