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A kind of complex of copper maleic dinitrile disulfide and preparation method thereof

A technology of dinitrile-based disulfide copper and copper complexes, which can be used in the preparation of thiols, organic chemistry, etc., and can solve the problems of less research on copper complexes.

Inactive Publication Date: 2016-07-06
NANYANG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Judging from the literature reports, domestic and foreign researchers have done a lot of research on maleic dinitrile disulfide nickel (III) complexes, while copper complexes have relatively little research.

Method used

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  • A kind of complex of copper maleic dinitrile disulfide and preparation method thereof
  • A kind of complex of copper maleic dinitrile disulfide and preparation method thereof
  • A kind of complex of copper maleic dinitrile disulfide and preparation method thereof

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Experimental program
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Embodiment 1

[0016] Copper chloride (0.0341g, 0.2mmol), Na 2 mnt (0.0742g, 0.4mmol) and [C 16 h 20 N 2 ] I 2 (0.0988g, 0.2mmol) was successively added to a round-bottomed flask containing 25mL of water, and stirred thoroughly for 2 hours; the precipitate was filtered, washed with water, and dried in vacuo. The precipitate was dissolved in 6mL of dimethylformamide, filtered, and the filtrate was transferred to a 25mL test tube, and diethyl ether was used as a poor solvent for diffusion. After three weeks, massive crystals were obtained, which were filtered and washed with water to obtain the target compound. Yield 19% (calculated based on Cu content). Molecular formula: C 24 h 20 CuN 6 S 4 , elemental analysis, calculated: C, 49.34; H, 3.45; N, 14.38. Found: C, 49.32; H, 3.46; N, 14.29.

Embodiment 2

[0018] Copper chloride (0.0341g, 0.2mmol), Na 2 mnt (0.0742g, 0.4mmol) and [C 16 h 20 N 2 ] I 2 (0.0988g, 0.2mmol) was successively added to a round-bottomed flask containing 25mL of water, and stirred thoroughly for 2 hours; the precipitate was filtered, washed with water, and dried in vacuo. The precipitate was dissolved in 9 mL of dimethylformamide, filtered, and the filtrate was transferred to a 25 mL test tube, and diethyl ether was used as a poor solvent for diffusion. After three weeks, blocky crystals were obtained, which were filtered and washed with water to obtain the target compound. Yield 28% (according to Cu content calculation). Molecular formula: C 24 h 20 CuN 6 S 4 , elemental analysis, calculated: C, 49.34; H, 3.45; N, 14.38. Found: C, 49.29; H, 3.41; N, 14.39.

Embodiment 3

[0020] Copper chloride (0.0341g, 0.2mmol), Na 2 mnt (0.0742g, 0.4mmol) and [C 16 h 20 N 2 ] I 2 (0.0988g, 0.2mmol) was successively added to a round-bottomed flask containing 25mL of water, and stirred thoroughly for 2 hours; the precipitate was filtered, washed with water, and dried in vacuo. The precipitate was dissolved in 12 mL of dimethylformamide, filtered, and the filtrate was transferred to a 25 mL test tube, and diethyl ether was used as a poor solvent for diffusion. After three weeks, massive crystals were obtained, which were filtered and washed with water to obtain the target compound. Yield 22% (according to Cu content calculation). Molecular formula: C 24 h 20 CuN 6 S 4 , elemental analysis, calculated: C, 49.34; H, 3.45; N, 14.38. Found: C, 49.30; H, 3.38; N, 14.40.

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Abstract

The invention relates to a copper maleonitriledithiolate (mnt) complex and a preparation method thereof. The maleonitrile copper dithiolate complex has a molecular formula of C24H20CuN6S4 and the molecular weight of 584.24. A synthesis method of the copper maleonitriledithiolate complex comprises the following steps: adding copper chloride, Na2mnt and [Cl6H20N2]I2 into a round-bottom flask containing 25ml of water in sequence, and sufficiently stirring for 2 hours; filtering to obtain precipitate, and washing the precipitate with water and drying in vacuum; and dissolving the precipitate in 6-12ml of dimethylformamide, filtering, transferring the filtrate to a 25mL test tube, dispersing with diethyl ether as a poor solvent for three weeks to obtain blocky crystals, filtering and washing the blocky crystals with water to obtain a target product.

Description

technical field [0001] The invention relates to a maleic dinitrile disulfide copper complex and a preparation method thereof. Provide theoretical basis and experimental basis for the rational design and synthesis of maleic dinitrile dithioene complexes with novel structures and excellent properties. Background technique [0002] Molecular materials have become the focus of attention in recent years because of their novel structures and potential applications in catalysis, electrical conduction, luminescence, magnetism and nonlinear optics. Once the ligands and their complexes with novel structures and unique functions appear, they will often set off a research boom, which will greatly promote related fields, open up new research directions, and promote interdisciplinary and integration. Malay Dinitrile dithioenes are one such ligand. (P.J.Hagrman, D.HagrmanandJ.Zubieta, Angew.Chem.Int.Ed., 1999,38,2638; C.Benelli, D.Gatteschi, Chem.Rev., 2002,102,2369; O.R.EvansandW.Lin, A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/54C07C319/12C07D213/127
Inventor 闫卫红申明乐姬鄂豫徐雪丽杜朝军
Owner NANYANG INST OF TECH