Pyrimidine-ring-contained palladium metal ligand and preparation method thereof

A metal ligand and pyrimidine-based ring technology, applied in the field of organic synthesis, can solve the problems of strong coordination ability and many coordination sites of multidentate ligands, and achieve the effects of stable structure, low requirements for reaction conditions, and convenient storage and transportation.

Inactive Publication Date: 2010-11-17
LUOYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, multi-dentate ligands have many coordination sites and strong coordination ability, and it is easy to genera

Method used

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  • Pyrimidine-ring-contained palladium metal ligand and preparation method thereof
  • Pyrimidine-ring-contained palladium metal ligand and preparation method thereof
  • Pyrimidine-ring-contained palladium metal ligand and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

Example 1

In the palladium metal ligand containing a pyrimidinyl ring,

among them:

Example Embodiment

Example 2

Preparation of 2,4-diphenylpyrimidinyl cyclopalladium metal ligand (1): under the protection of an inert gas (such as high-purity nitrogen), to a 10rh Schlek reaction tube (a commonly used in anhydrous and oxygen-free operation) Glassware) add 0.5mmol 2-phenyl-4-chloropyrimidinyl cyclopalladium triphenyltriphenyl adduct, 0.6mmol phenylboric acid, 1mmol potassium carbonate, replace the reaction tube with nitrogen 3 times, and press Under the continuous protection of nitrogen, 5ml of toluene solvent was added with a syringe, and then heated to 110°C in an oil bath under magnetic stirring, and the reaction was refluxed for 12 hours.

After the reaction, the oil bath was removed, and the water bath was lowered to room temperature; 3ml of water was added to the reaction solution, and then extracted three times with 5ml of dichloromethane. The organic phases were combined and used anhydrous MgSO 4 Dry for 30 minutes and filter; the filtrate is concentrated on a rotary evapor...

Example Embodiment

Example 3

Preparation of 2-(2-methylphenyl)-4-(2-pyridinyl)pyrimidinyl ring palladium metal ligand (3): Under nitrogen protection, add 0.5mmol 2-(2) to a 10rh Schlek reaction tube -Methylphenyl)-4-bromopyrimidinyl cyclopalladium triphenylene adduct, 0.5mmol of 2-pyridylboronic acid, 0.5mmol of sodium carbonate; replace the reaction tube with nitrogen 3 times, and under a slight positive pressure of nitrogen Add 5ml of dioxane solvent with a syringe under the continuous protection of, and heat to 90℃ with an oil bath under magnetic stirring, and the reaction will be refluxed for 8 hours.

After the reaction, the oil bath was removed, and the water bath was lowered to room temperature; 3ml of water was added to the reaction solution, and then extracted three times with 5ml of dichloromethane. The organic phases were combined and used anhydrous MgSO 4 Dry for 30 minutes and filter; the filtrate is concentrated with a rotary evaporator, and the concentrated residue is separated by s...

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Abstract

The invention relates to a pyrimidine-ring-contained palladium metal ligand and a preparation method thereof, belonging to the field of organic synthesis. The pyrimidine-ring-contained palladium metal ligand has a general formula which is shown in the specification, wherein the dotted portion is R; R is aryl or ferrocenyl, R1 is phenyl, ring ethyl, ethyl, propyl, or butyl, and Aryl is aryl or heterocyclic group, and X is selected from Cl-, Br- and I-. The preparation method of the pyrimidine-ring-contained palladium metal ligand comprises the following steps of: mixing halogenated pyrimidine ground ring single palladium adduct, Aryl-B(OH)2, alkali and organic solvent; heating and refluxing under the protection of inert gases; adding water after refluence; and then, adding an organic solvent to extract products to obtain a pyrimidine-ring-contained palladium metal ligand. The halogenated pyrimidine ground ring single palladium adduct has a general formula which is shown in the specification, wherein the dotted portion is R; the X1 is Cl-, Br- or I-. The method avoids the direct reaction between a multidentate ligand and a palladium source, avoids adding an additional palladium catalyst in a reaction process, has low requirements for reaction conditions, high yield and stable products and can be used for preparing ring-palladium polynuclear metal compositions.

Description

technical field The invention belongs to the field of organic synthesis, and in particular relates to a class of pyrimidinyl-containing ring palladium metal ligands, and also relates to a preparation method of the compounds. Background technique In recent years, heteropolynuclear metal complexes have outstanding performance in the fields of magnetic exchange of metal ions, electron transfer, bioinorganic chemistry, etc., and have developed into a hot research field, especially in the research of new high-efficiency catalysts and special materials. application. At present, the synthesis methods of heteropolynuclear metal complexes mainly include the following: (1) polymerization of mononuclear complexes; (2) synthesis of complexes as ligands; (3) synthesis by multidentate ligands; (4) Directly synthesized by polyatomic bridging groups; (5) synthesized by substitution reaction of metal ions; (6) spontaneously self-assembled. Among them, the method of "using complexes as liga...

Claims

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Application Information

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IPC IPC(8): C07F19/00C07F15/00C07F17/02B01J31/24
Inventor 徐晨高辉刘辉娄新华李红梅王志强
Owner LUOYANG NORMAL UNIV
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