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Synthesis method and application of flexible carboxylic acid and transition metal complex

A technology of transition metal and synthesis method, which is applied in the application field of catalyzing the hydroxylation of phenol, and can solve the problems of less research on flexible carboxylic acid ligands and the like

Inactive Publication Date: 2014-02-19
宣城明美蓝莓科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the carboxylic acid complexes that have been synthesized at present are complexes with rigid carboxylic acid ligands, and there are relatively few studies on flexible carboxylic acid ligands.

Method used

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  • Synthesis method and application of flexible carboxylic acid and transition metal complex
  • Synthesis method and application of flexible carboxylic acid and transition metal complex
  • Synthesis method and application of flexible carboxylic acid and transition metal complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 95wt% ethanol to the reaction kettle containing the organic ligand 5-amino-1,2,4-triazole-3-carboxylic acid to dissolve completely,

[0025] (2) Prepare an aqueous solution of lead tetrafluoroborate with a concentration of 50wt%,

[0026] (3) By solvothermal method, according to the molar ratio of metal salt to organic ligand 1:1, add the metal salt solution to the organic ligand solution obtained in step (1) and mix well, adjust the pH to 3-5, heat to 160°C and Boil at constant temperature for 48 hours, cool down to room temperature, wash and filter to obtain colorless needle-like crystals, labeled as complex 1. The infrared spectrum of the complex is shown in figure 1 shown by figure 1 It can be seen that 3430 cm -1 Absorption peaks appear within the range, indicating that crystal water exists in the complex. at 1720-1680 cm -1 There is no absorption peak in the range, indicating that the carboxyl group COOH has been completely deprotonated.

Embodiment 2

[0028] The organic ligand is adipic acid, the metal salt is lead nitrate, the other processes are the same as in Example 1, and a colorless block crystal is obtained, which is marked as complex 2. The infrared spectrum of the complex is shown in figure 2 As can be seen from the figure, 3430 cm -1 A broad absorption peak appears in the range, indicating that there is coordination water or crystal water in the complex. at 1720-1680 cm -1 There is no absorption peak in the range, indicating that the carboxyl COOH has been completely deprotonated.

Embodiment 3

[0030] The organic ligand is 2,3-quinoline dicarboxylic acid, the metal salt is lead nitrate, the other processes are the same as in Example 1, and light yellow needle-like crystals are obtained, which are marked as complex 3. The infrared spectrum of the complex is shown in image 3 Shown, as can be seen from the figure, 3300-3500 cm -1 Absorption peaks appear within the range, indicating that coordination water or crystal water exists in the complex. at 1720-1680 cm -1 There is no absorption peak in the range, indicating that the carboxyl COOH has been completely deprotonated. 1540cm -1 It is C=O stretching vibration.

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Abstract

The invention discloses a method for synthesizing a flexible carboxylic acid and transition metal complex by taking Fe<3+>, Pb<2+> or Ba<2+> as a metal center and the 5-amino-1,2,4-triazole-3-carboxylic acid, succinic acid, malonic acid, adipic acid, butenedioic acid (cis, trans), 2,3-quinoline dicarboxylic acid or 2,5-dicarboxythiophene as an organic ligand, and provides an application of the complex serving as a catalyst to catalyze a phenol hydroxylation reaction. Through the method and application disclosed by the invention, by taking the synthesized complex as a catalyst to catalyze the phenol hydroxylation to obtain benzenediol, the yield can approach 74%; and the catalysis reaction is green and environment-friendly, and the catalyst is expected to become a novel catalyst for catalyzing phenol hydroxylation.

Description

technical field [0001] The invention relates to a synthesis method of a complex of a flexible carboxylic acid and a transition metal and the application of the complex as a catalyst in catalyzing the hydroxylation of phenol. Background technique [0002] Since the founding of coordination chemistry by A. Werner for a century, coordination chemistry has been continuously enriched and developed under the unremitting efforts of generations of scientific researchers. Among them, the research on coordination polymers is also one of the frontiers in the development of coordination chemistry. Coordination polymer refers to a skeleton compound with a network three-dimensional structure formed by organic ligands and metal ions through weak forces such as coordination bonds, hydrogen bonds, π-π interactions, and van der Waals forces. Coordination polymers have diverse topological structures and excellent physical and chemical properties, and have good potential application prospects ...

Claims

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Application Information

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IPC IPC(8): C07F15/02C07F7/24C07F3/00B01J31/22C07C37/60C07C39/08
Inventor 董华泽伍颖搏
Owner 宣城明美蓝莓科技有限公司
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