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

Bis-nitroheterocyclic carbene bis-palladium complex and preparation method thereof

A technology of diazide heterocycle and palladium complex is applied in the field of double palladium complex and its preparation, can solve the problems of easy decomposition of synthesis steps, waste of silver and the like, and achieves the effects of simple synthesis method, high yield and convenient post-processing

Inactive Publication Date: 2011-12-14
XUZHOU NORMAL UNIVERSITY
View PDF2 Cites 14 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is widely used, but there are several disadvantages: (1) silver oxide is easy to decompose when exposed to light (2) the synthesis steps are long (3) a lot of silver is wasted in the reaction, etc.

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
  • Bis-nitroheterocyclic carbene bis-palladium complex and preparation method thereof
  • Bis-nitroheterocyclic carbene bis-palladium complex and preparation method thereof
  • Bis-nitroheterocyclic carbene bis-palladium complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: L 1a (PdCl 2 ) 2 (Py) 2 Synthesis and Characterization of Binuclear Palladium Metal Compounds

[0027]

[0028] Add (L 1a ) 1,1'-di-trimethylphenyl-3,3'-(1,2-ethylene)diimidazole dichloride (1.414g, 3mmol), PdCl 2 (1.069g, 6.0mmol), K 2 CO 3 (8.293g, 60mmol), add a condenser and turn the cap on the condenser orifice. Ventilate the air three times on the vacuum line to ensure that the system is filled with argon. Use a syringe to take 35.5 mL of anhydrous treated pyridine and add it to the reactor. Insert a balloon filled with argon on the system opening plug and add it to the oil bath. Reaction at 85°C for 18h. After the reaction was completed, the reaction solution was passed through celite, washed with dichloromethane, and the filtrate was collected. The solvent was distilled off under reduced pressure to obtain a yellow crude product, 2.27 g of a light yellow solid recrystallized from dichloromethane / ether, with a yield of 83%.

[0029] 1 H N...

Embodiment 2

[0030] Example 2: L 1b (PdCl 2 ) 2 (Py) 2 Synthesis and Characterization of Binuclear Palladium Metal Compounds

[0031]

[0032] Add (L 1b ) 1,1'-di-me-trimethylphenyl-3,3'-(1,3-propylene) diimidazole dichloride (1.457g, 3mmol), PdCl 2(1.069g, 6.0mmol), and K 2 CO 3 (8.293g, 60mmol), add a condenser and turn the cap on the condenser orifice. Ventilate the air three times on the vacuum line to ensure that the system is filled with argon. Use a syringe to take 35.5 mL of anhydrous treated pyridine and add it to the reactor. Insert a balloon filled with argon on the system opening plug and add it to the oil bath. Reaction at 85°C for 18h. After the reaction was completed, the reaction solution was passed through celite, washed with dichloromethane, and the filtrate was collected. The solvent was distilled off under reduced pressure to obtain a yellow crude product, 2.142 g of a light yellow solid recrystallized from dichloromethane / ether, with a yield of 77%.

[003...

Embodiment 3

[0034] Example 3: L 1c (PdCl 2 ) 2 (Py) 2 Synthesis and Characterization of Binuclear Palladium Metal Compounds

[0035]

[0036] Add (L 1c ) 1,1'-di-me-trimethylphenyl-3,3'-(1,4-butylene)diimidazole dichloride (1.499g, 3mmol), PdCl 2 (1.069g, 6.0mmol), and K 2 CO 3 (8.293g, 60mmol), add a condenser and turn the cap on the condenser orifice. Ventilate the air three times on the vacuum line to ensure that the system is filled with argon. Use a syringe to take 35.5 mL of anhydrous treated pyridine and add it to the reactor. Insert a balloon filled with argon on the system opening plug and add it to the oil bath. Reaction at 85°C for 18h. After the reaction was completed, the reaction solution was passed through celite, washed with dichloromethane, and the filtrate was collected. The solvent was distilled off under reduced pressure to obtain a yellow crude product, 1.807 g of a pale yellow solid recrystallized from dichloromethane / ether, with a yield of 64%.

[0037]...

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 bis-nitrogen heterocyclic carbene bis-palladium complex and a preparation method thereof, which belong to the bis-palladium complex and a preparation method thereof. The preparation method is as follows: according to the molar ratio of 1:2.05:20, bis-imidazolium chloride salt, palladium chloride, and potassium carbonate are added into a round-bottomed flask, a condenser is added to the mouth of the flask, and an inversion plug is added to the condenser. Connect it to a double-row tube vacuum line connected with argon; react at 85°C for 18h; Wash the diatomaceous earth until no yellow liquid flows down, and collect the filtrate; use a rotary evaporator to remove dichloromethane in the collected filtrate, and remove pyridine in the collected filtrate to obtain a yellow crude product; recrystallize with dichloromethane / ether to obtain a light yellow solid , that is, the bis-palladium complex of the diazoheterocyclic carbene is obtained. The synthesis step of the invention is simple, the yield is high, and it is convenient to realize industrialization.

Description

technical field [0001] The invention relates to a double palladium complex and a preparation method thereof, in particular to a diazaheterocyclic carbene double palladium complex and a preparation method thereof. Background technique [0002] Homogeneous catalysis has become one of the rapidly developing fields in chemistry, and highly active catalysts can complete reactions quickly and with high yields. Nitrogen-heterocyclic carbene palladium complexes are a kind of good catalysts. They have been used in a certain range in organic synthesis and homogeneous catalysis. Nitrogen-containing heterocyclic carbene palladium complexes can catalyze C-C, C-N, C-S and other bonds. Formation. The known nitrogen heterocyclic carbene palladium complexes can be roughly divided into the following four categories: 1. Monocarbene monometallic palladium complexes, which have been extensively studied. 2. Double carbene single metal palladium complexes, which can be further divided into compl...

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
IPC IPC(8): C07F15/00B01J31/22
Inventor 史延慧曹昌盛庄永忠
Owner XUZHOU NORMAL UNIVERSITY
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