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Process of preparing 2-thio benzothiazole transition metal cluster compound

A mercaptobenzothiazole and transition metal technology is applied in the field of preparing 2-mercaptobenzothiazole transition metal clusters, and can solve the problems of affecting application promotion, low solubility and the like

Inactive Publication Date: 2006-11-15
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the low solubility of these clusters in common organic solvents seriously hinders their popularization.

Method used

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  • Process of preparing 2-thio benzothiazole transition metal cluster compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1: Synthesis of 2-mercaptobenzothiazolium iron clusters

[0012] In a 250mL three-necked flask equipped with a thermometer, a reflux condenser and a stirring magnet, add 4.00g (0.024mol) of 2-mercaptobenzothiazole and 80mL of absolute ethanol, and stir to completely dissolve the solid. Then, 1.70 g (0.025 mol) of sodium ethoxide was added, and stirring was continued for 8 hours, followed by the dropwise addition of 50 mL of 30% FeSO 4 Aqueous solution, control the temperature of the system at reflux temperature, stir for 1 hour, a yellow-brown precipitate is formed, cool to room temperature, filter, wash the yellow-brown precipitate with water, and dry at a temperature lower than 100°C to obtain yellow-brown 2-mercaptobenzothiazole Iron cluster crystals, yield 3.08g (yield about 62.3%).

[0013] The physical and spectroscopic properties of the obtained compound are as follows:

[0014] Melting point: 273-275°C.

[0015] Elemental analysis: theoretical value C...

Embodiment 2

[0017] Example 2: Synthesis of 2-mercaptobenzothiazole cobalt clusters

[0018] In a 250mL three-necked flask equipped with a thermometer, a reflux condenser and a stirring magnet, add 4.00g (0.024mol) of 2-mercaptobenzothiazole and 80mL of absolute ethanol, and stir to completely dissolve the solid. Then, 1.70 g (0.025 mol) of sodium ethoxide was added, and stirring was continued for 7 hours, followed by the dropwise addition of 50 mL of 30% CoCl 2 Aqueous solution, control the temperature of the system at reflux temperature, stir for 1.5 hours to form a green precipitate, cool to room temperature, filter, wash the green precipitate with water, and dry it below 100°C to obtain a green 2-mercaptobenzothiazole cobalt cluster Compound crystals, yield 3.07g (yield about 61.4%).

[0019] The physical and spectroscopic properties of the obtained compound are as follows:

[0020] Melting point: 311-312°C.

[0021] Elemental analysis: theoretical value C 42 h 24 N 6 co 4 OS 1...

Embodiment 3

[0023] Embodiment 3: the synthesis of 2-mercaptobenzothiazole nickel cluster compound

[0024] In a 250mL three-necked flask equipped with a thermometer, a reflux condenser and a stirring magnet, add 4.00g (0.024mol) of 2-mercaptobenzothiazole and 80mL of absolute ethanol, and stir to completely dissolve the solid. Then, 1.70 g (0.025 mol) of sodium ethoxide was added, and stirring was continued for 7 hours, followed by the dropwise addition of 50 mL of 30% NiSO 4 Aqueous solution, control the temperature of the system at reflux temperature, stir for 1 hour, a purple precipitate is formed, cool to room temperature, filter, wash the purple precipitate with water, dry below 100°C, and obtain a purple 2-mercaptobenzothiazole nickel cluster Compound crystals, yield 3.16g (yield about 63.3%).

[0025] The physical and spectroscopic properties of the obtained compound are as follows:

[0026] Melting point: 332-334°C.

[0027] Elemental analysis: theoretical value C 42 h 24 N ...

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Abstract

A process for preparing the 2-mercapto benzothiazole cluster compound of transition metals features use of 'reflux method' with high output rate. Said cluster compound can be used for non-linear optical material and sulfurizing promoter.

Description

Technical field: [0001] The present invention relates to a novel process for the preparation of 2-mercaptobenzothiazole transition metal clusters. This product is an ideal nonlinear optical material and can be used as a rubber vulcanization accelerator. Background technique: [0002] Metal atom cluster compound is a kind of metal-metal bonding or metal-bridge bonding, so that adjacent metal atoms or metal centers containing ligands are connected together with two or more metal atoms. Because metal clusters are closely related to metal catalysts, and they are active centers that play an important role in biological enzymes and biological proteins, and the rich and colorful physical and chemical properties determined by the peculiar and changeable structures of metal clusters are constantly being revealed. , and their possibility as binary and ternary materials have been recognized, so that the chemical research of metal atomic clusters continues to deepen. For a long time, ...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 建方方赵朴素李颖
Owner QINGDAO UNIV OF SCI & TECH
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