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Application of ammonium thiosulfate as reducing agent in preparation of 5-amino-1,10-phenanthroline

A technology of ammonium thiosulfate and phenanthroline, applied in the chemical industry, can solve the problems of environmental pollution, low cost, unfavorable operators and the environment, etc., and achieves the effects of simple and convenient operation and simple equipment

Inactive Publication Date: 2013-07-03
NANJING UNIV OF INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkali sulfide reduction method has low cost, but its reduction efficiency is not high, and harmful gas is released during the reaction, which is not good for the operator and the environment
The above methods are limited because they will cause serious environmental pollution, prompting people to explore new and more environmentally and economically beneficial production methods

Method used

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  • Application of ammonium thiosulfate as reducing agent in preparation of 5-amino-1,10-phenanthroline

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] In a four-neck flask, add 1 g of compound (1): 5-nitro-1,10-phenanthroline. Then 20ml of ethanol and 10ml of water were added. Start heating and stirring. After the compound is completely dissolved, add 6g of 96.1% (NH 4 ) 2 S 2 o 3 . Let it all dissolve. The reaction was refluxed at 80° C. for 4 hours. After 4 hours, cool to room temperature naturally. A yellow flake compound was precipitated, and the precipitated compound was filtered out with suction. Compound (2): 5-amino-1,10-phenanthroline was obtained after complete drying. The weighed weight was 0.73 g. The yield is about 84.2%.

example 2

[0023] In a four-neck flask, add 1 g of compound (1): 5-nitro-1,10-phenanthroline. Then 80ml of ethanol and 40ml of water were added. Start heating and stirring. After the compound is completely dissolved, add 6g of 96.1% (NH 4 ) 2 S 2 o 3 . Let it all dissolve. The reaction was refluxed at 80° C. for 4 hours. After 4 hours, cool to room temperature naturally. A yellow flake compound was precipitated, and the precipitated compound was filtered out with suction. Compound (2): 5-amino-1,10-phenanthroline was obtained after complete drying. The weighed weight was 0.68g. The yield is about 78.4%.

example 3

[0025] In a four-neck flask, add 1 g of compound (1): 5-nitro-1,10-phenanthroline. Then 200ml of ethanol and 80ml of water were added. Start heating and stirring. After the compound is completely dissolved, add 6g of 96.1% (NH 4 ) 2 S 2 o 3 . Let it all dissolve. The reaction was refluxed at 80° C. for 4 hours. After 4 hours, cool to room temperature naturally. A yellow flake compound was precipitated, and the precipitated compound was filtered out with suction. Compound (2): 5-amino-1,10-phenanthroline was obtained after complete drying. The weighed weight was 0.70 g. The yield is about 80.7%.

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Abstract

The invention discloses a new purpose of ammonium thiosulfate as a reducing agent in the preparation of 5-amino-1,10-phenanthroline. The operation steps are as follows: adding an organic solvent and water into 5-nitro-1,10-phenanthroline, wherein 20-200ml of the organic solvent is added into each gram of the 5-nitro-1,10-phenanthroline; adding 10-80ml of water into each gram of the 5-nitro-1,10-phenanthroline; further adding the ammonium thiosulfate according the proportion of adding 1-50g of the ammonium thiosulfate into each gram of the 5-nitro-1,10-phenanthroline, mixing, then heating to 30 DEG C to 80 DEG C, performing reflux reaction for 4-48h, then cooling to room temperature, precipitating solids, and performing suction filtration and drying on a precipitate to get the 5-amino-1,10-phenanthroline. The technical scheme disclosed by the invention has the advantages of simplicity and convenience in the operation of the method, no production of environmental pollution and simple equipment, and is suitable for continuous production.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and specifically relates to the application and use method of ammonium thiosulfate as a reducing agent in the preparation of 5-amino-1,10-phenanthroline. Background technique [0002] 1,10-Phenanthroline and its derivatives have good coordination properties, so they play an important role not only in crystallography but also in many fields. Now it has become a widely used chelating ligand. For example, it is an important chelating agent in chemical analysis and catalytic chemistry; its complexes are important electron transfer agents in life science research, etc. Used in the preparation of rare earth metal chelates to develop organic electroluminescent / photoluminescent materials. It is also an important organic synthesis intermediate. [0003] 5-Amino-1,10-phenanthroline is an important chemical raw material, which is widely used in dyestuffs, pharmaceuticals, agricultural chemicals...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
Inventor 张超智孙晓飞张骁胡鹏李世娟沈丹
Owner NANJING UNIV OF INFORMATION SCI & TECH