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Preparation of sulfide-containing metal complex

A technology of metal complexes and thioether compounds, applied in the direction of organic chemistry, can solve the problems of limited types, and achieve the effects of strong applicability, wide sources, and low toxicity

Inactive Publication Date: 2009-01-21
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In the above-mentioned prior art, the alkyl group added to the S atom comes from a halogenated alkane or alkene, and its type is limited by the type of a halogenated alkane or alkene

Method used

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  • Preparation of sulfide-containing metal complex
  • Preparation of sulfide-containing metal complex
  • Preparation of sulfide-containing metal complex

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment one: see attached figure 1 , a kind of preparation method that contains sulfide metal complex, comprises the following steps:

[0031] (1) 0.05 mmol cadmium iodide (CdI 2 ), 0.05 mmol iodine (I 2 ), 0.05 mmol 4-mercaptopyridine (C 5 h 5 NS) and 1 milliliter of methanol are reaction starters, mixed in 1 milliliter of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;

[0032] (2) Then slowly lower the temperature to obtain a colorless solution. The solution was evaporated and concentrated at room temperature to obtain colorless blocky crystals. Its single crystal structure (C 7 h 10 NS) 2 (CdI 4 )Such as figure 1 As shown, the methyl group on methanol is transferred to the S and N of 4-mercaptopyridine to form (C 7 h 10 NS) + Cation, anion is (CdI 4 ) 2- tetrahedron.

[0033] (3) The crystalline product is enriched by filtration, washed once with 2 ml of acetonitrile, and washed three times with 2 ml of ether respect...

Embodiment 2

[0035] Embodiment two: see attached figure 2 , a kind of preparation method that contains sulfide metal complex, comprises the following steps:

[0036] (1) 0.05 mmol of cuprous iodide (CuI), 0.05 mmol of iodine (I 2 ), 0.05 mmol 4-mercaptopyridine (C 5 h 5 NS) and 1 milliliter of methanol are reaction starters, mixed in 1 milliliter of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;

[0037] (2) Slowly lower the temperature to obtain a brown-yellow solution. The solution was naturally evaporated and concentrated at room temperature to obtain yellow blocky crystals. Its single crystal structure (C 7 h 10 NS) 2 (Cu 2 I 4 )Such as figure 2 As shown, the methyl group on methanol is transferred to the S and N of 4-mercaptopyridine to form (C 7 h 10 NS) + Cations, anions are (Cu 2 I 4 ) 2- dimer. At the same time, the S atom on the generated thioether coordinates with the Cu atom.

[0038] (3) The crystalline product is enriched by...

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Abstract

The invention discloses a method for preparing a sulfur-aether contained metal complex. The method is characterized in that a simpler substance of iodine, metal iodides, an alcohol, and 4-mercaptopyridine are mixed with acetonitrile and react under a solvothermal condition to transfer the alkyl group on the alcohol to a sulfur atom of a mercapto compound to produce a sulfur-aether compound; because of the possibility to synthesize the sulfur-aether contained metal complex containing various metals through the changing of alcohols and the metal iodides, the method for preparing the sulfur-aether contained metal complex provided by the invention has high applicability; additionally, various kinds of sulfur-aether compound can be produced, because of both the relatively low toxicity of ethanol as the raw material providing the alkyl group, and more categories of alcohols available compared with haloalkanes or alkene.

Description

technical field [0001] The invention relates to a preparation method of a sulfide-containing metal complex. Background technique [0002] Thioether compounds are important reaction raw materials and reagents in the chemical industry, and it is of great significance to explore the synthesis methods of such compounds. [0003] The preparation method of existing thioether compound mainly contains three kinds: [0004] (1) Prepared by the alkylation reaction of mercaptan: [0005] R-Br+HS-R'→R-S-R'+HBr [0006] Alkali can catalyze this kind of reaction, and the mechanism is to generate a mercaptide with stronger nucleophilicity, and the thioether prepared by this method is generally an asymmetric thioether. [0007] (2) The reaction of mercaptans and olefins can also produce thioethers, which are catalyzed by free radicals: [0008] R-CH=CH2+HS-R'→R-CH2-CH2-S-R' [0009] In this series of reactions, in the presence of peroxides, thiols or thiophenols undergo free radical ad...

Claims

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Application Information

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IPC IPC(8): C07D213/70
Inventor 郎建平陈阳程美令任志刚魏振宏黎玲玲
Owner SUZHOU UNIV
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