Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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

A technology of metal ligands and pyrimidinyl rings, which is applied in the field of organic synthesis, can solve the problems of strong coordination ability and multi-dentate ligand coordination sites, and achieve the effects of stable structure, low requirements for reaction conditions, and convenient storage and transportation

Inactive Publication Date: 2013-07-17
LUOYANG NORMAL UNIV
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, multi-dentate ligands have many coordination sites and strong coordination ability, and it is easy to generate palladium complexes instead of the required cyclopalladium compounds when directly reacting with palladium sources.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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

Embodiment 1

[0023] Containing pyrimidinyl cyclopalladium metal ligands, the general formula is:

[0024] Where the dashed part is R:

[0025]

Embodiment 2

[0027] 2, the preparation of 4-diphenylpyrimidinyl cyclopalladium metal ligand (1): under the protection of an inert gas (such as high-purity nitrogen), the Schlek reaction tube (a kind of commonly used during anhydrous and anaerobic operation) of 10ml Glass instrument) add 0.5mmol 2-phenyl-4-chloropyrimidinyl cyclopalladium triphenylsulfone adduct, 0.6mmol phenylboronic acid, 1mmol potassium carbonate, replace the reaction tube with nitrogen for 3 times, and Under the continuous protection of nitrogen, 5ml of toluene solvent was added with a syringe, and then heated to 110°C with an oil bath under magnetic stirring, and the reaction was refluxed for 12 hours.

[0028] 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 washed with anhydrous MgSO 4 Dry for 30 minutes and filter; the filtr...

Embodiment 3

[0030] Preparation of 2-(2-methylphenyl)-4-(2-pyridyl)pyrimidinyl cyclopalladium metal ligand (3): under nitrogen protection, add 0.5mmol 2-(2 -Methylphenyl)-4-bromopyrimidinyl cyclopalladium triphenylsulfone adduct, 0.5mmol of 2-pyridylboronic acid, 0.5mmol of sodium carbonate; replace the reaction tube with nitrogen for 3 times, and in slight positive pressure nitrogen Add 5ml of dioxane solvent with a syringe under the continuous protection of ; heat to 90°C with an oil bath under magnetic stirring, and reflux the reaction for 8 hours.

[0031] 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 washed with anhydrous MgSO 4 Dry for 30 minutes and filter; the filtrate is concentrated by a rotary evaporator, and the concentrated residue is separated by silica gel thin-layer chromatograph...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 [0001] 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 [0002] 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 c...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com