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Synthetic method of mixed ligand coordination planar metal disulfide ene complex

A technology of mixing ligands and disulfides, which can be applied to gold-organic compounds, 1/11 group organic compounds without C-metal bonds, nickel-organic compounds, etc., can solve problems such as difficulty in synthesizing metal disulfide complexes

Active Publication Date: 2015-09-23
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common metal dithioene ligands such as dmit, mnt, dddt, dtcr, etc. all belong to ligands with electron-withdrawing structure, and the synthesis of metal dithioene complexes with mixed coordination between these ligands is relatively difficult.

Method used

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  • Synthetic method of mixed ligand coordination planar metal disulfide ene complex
  • Synthetic method of mixed ligand coordination planar metal disulfide ene complex
  • Synthetic method of mixed ligand coordination planar metal disulfide ene complex

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Complex [Ni(dtcr)(mnt)](Bu 4 N) 2 Synthesis

[0054] (1) Add o-phenanthroline (2.2g) and NiCl in a 250mL flask 2 ·6H 2 O (1.2g) was dissolved in 50mL 95% ethanol solution, after mixing and stirring uniformly, a light purple solution was obtained, 1.25g pentasquarate sulfur potassium (dtcr) was weighed and dissolved in 30mL water and added to the above solution, the solution became dark purple, Control the temperature at 70-80°C and stir for 30 minutes to obtain an insoluble black solid, which is filtered and washed three times with 10 mL of ethanol and water respectively;

[0055] (2) The tetrabutylammonium bromide salt of the solid that step (1) obtains and the 1.2g maleic dinitrile potassium disulfate (mnt), 1.0g KOH and 3.5g are mixed, add 350mL water, in Stir and heat to boiling, stop the reaction after 300mL of liquid is evaporated, after cooling, filter the solid and wash with 10mL of ice water for 3 times;

[0056] (3) Add 100 mL of acetone to the solid obta...

Embodiment 2

[0058] Complex [Ni(dtcr)(dcmdtcr)](Bu 4 N) 2 Synthesis

[0059] (1) Add o-phenanthroline (2.2g) and NiCl in a 250mL flask 2 ·6H 2O (1.2g) was dissolved in 50mL 95% ethanol solution, after mixing and stirring uniformly, a light purple solution was obtained, 1.25g pentasquarate sulfur potassium (dtcr) was weighed and dissolved in 30mL water and added to the above solution, the solution became dark purple, Control the temperature at 70-80°C and stir for 30 minutes to obtain an insoluble black solid, which is filtered and washed three times with 10 mL of ethanol and water respectively;

[0060] (2) The solid that step (1) obtains and the 1.5g dicyano-substituted sulfur potassium pentasquarate (dcmdtcr), 1.0g K 2 CO 3 Mix with 3.5g of tetrabutylammonium bromide salt, add 350mL of water, stir and heat to boiling, evaporate 300mL of liquid, stop the reaction, after cooling, filter the solid and wash with 10mL of ice water for 3 times;

[0061] (3) Add 100 mL of acetone to the s...

Embodiment 3

[0063] Complex [Ni(dtcr)(dmit)](Bu 4 N) 2 Synthesis

[0064] (1) Add 1,2-ethylenediamine (1.0mL) and NiCl to a 250mL flask 2 ·6H 2 O (1.2g) was dissolved in 50mL 95% ethanol solution, mixed and stirred evenly to obtain a light purple solution;

[0065] (2) Weigh 2.0g of dibenzoyl-substituted dmit ligand and add it to 50ml of newly configured sodium methoxide solution (50mL of methanol reacts with 1.0g of sodium metal), and after magnetic stirring for 30 minutes, filter the solution with absorbent cotton to step ( 1) in the solution, control the temperature at 70-80°C and stir for 30 minutes, and react to obtain an insoluble black solid, which is filtered and washed three times with 10 mL of ethanol and water respectively;

[0066] (3) the solid that step (2) obtains and the 1.25g potassium pentasquarate sulfur potassium (dtcr) that takes by weighing and the tetrabutylammonium bromide salt (Bu) of 3.5g 4 NBr) mixed, added 300mL of water, stirred and heated to boiling, stop...

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Abstract

The invention discloses a synthetic method of mixed ligand coordination planar metal disulfide ene complex and particular relates to synthesis of mixed ligand coordination planar complex of two metal disulfide ene ligands with the similar electron push and pull capability. The method comprises the following steps that 95% of ethanol solution of N,N double-tooth cheland is added into a flask, a water solution with metal ionicsalt is slowly added into the flask, after even mixing and stirring, metal disulfide ene ligand L1 is weighed and dissolved in the solution, stirring is conducted for 30 minutes at the temperature from 70 DEG C to 80 DEG C, solid is filtered out of reaction solution and is washed through 10 mL of ethyl alcohol and water for three times; the obtained solid, the metal disulfide ene ligand L2, inorganic base and tetra-alkyl ammonium salt or kylphosphonium salt are mixed, 300-350 mL of water is added, stirring and heating is conducted, 250-300 mL of liquid is steamed out, then the reaction is stopped, and after being cooled, the solid is filtered out and washed through 10 mL of ice water for three times; organic solvent is added into the obtained solid for extraction, extraction liquid slowly volatilizes, and high-purity L1 and L2 ligand mixed coordination metal disulfide ene crystal can be precipitated.

Description

technical field [0001] The invention relates to a synthesis method of a mixed-ligand coordination planar metal disulfide complex, which belongs to the field of inorganic synthesis. Background technique [0002] Metal disulfide complexes belong to metal complex near-infrared dyes. These compounds have high thermal stability and near-infrared absorption properties, and are widely used in the fields of laser protection, electrophotography, and optical recording. Common metallodithioene ligands such as figure 1 shown. With respect to the plane d of the symmetric coordination 8 Metal disulfide complexes (such as figure 2 shown), the mixed ligand coordination plane d 8 Metal disulfide complexes (such as image 3 Shown) Due to the different push-pull electronic properties of the ligands on both sides of the central metal, it exhibits more abundant optical, electrical and magnetic properties. The absorption of metal disulfide complexes in the near-infrared band is derived fro...

Claims

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Application Information

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IPC IPC(8): C07F15/04C07F1/08C07F15/00C07F1/12
CPCC07F1/005C07F15/0066C07F15/045
Inventor 陈红余李平秦坤张熙曼
Owner TAISHAN MEDICAL UNIV
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