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
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  • 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 w

Method used

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  • 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]...

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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

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Application Information

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