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Synthesis method of bis-(N-(7-hydroxy-8-methyl-5-phenylphenazine-3-subunit)dimethylammonium)sulfate

A technology of phenylphenazine and dimethylammonium is applied in the field of compound preparation and achieves the effects of high yield, low cost and high product purity

Inactive Publication Date: 2013-05-15
HUBEI LINGZHI CHEM SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for the synthesis of bis(N-(7-hydroxyl-8-methyl-5-phenylphenazin-3-ylidene) dimethylammonium) sulfate which is not relevant at home and abroad. A kind of synthetic method of bis(N-(7-hydroxyl-8-methyl-5-phenylphenazine-3-ylidene) dimethyl ammonium) sulfate of acidic copper plating additive overcomes the technology of acidic copper plating additive bottleneck

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  • Synthesis method of bis-(N-(7-hydroxy-8-methyl-5-phenylphenazine-3-subunit)dimethylammonium)sulfate

Examples

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Effect test

Embodiment 1

[0014] Example 1: Add 108g of p-hydroxy-m-toluidine, 123g of N,N-dimethylaniline, 250g of hydrochloric acid, and 200g of water into a 1000ml three-neck flask, cool to about 15°C, stir, and pass air at a pressure of 0.01-0.02Mpa 5 hour, then add aniline 95g, 100g hydrochloric acid into the three-necked flask, ventilate the air for 5 hours, after ventilating, add 109g sodium carbonate, add saturated sodium chloride solution 200 ml, let stand and separate layers, the upper layer is viscous, and the lower layer is Water layer, separate to remove the water layer; add 200ml of ethanol to the viscous material in the upper layer, stir and let stand for half an hour, remove the upper layer, and add 50% H 2 SO 4 A total of 98g was vacuum dehydrated and dried to obtain 110g of the product. After detection by liquid chromatography, the content is 85%, and the yield is 53.7%.

Embodiment 2

[0015] Example 2: 108g of p-hydroxy-m-toluidine, 123g of N,N-dimethylaniline, 250g of hydrochloric acid, and 200g of water were added to a 1000ml three-neck flask, cooled to about 10°C, stirred, and 200g of sodium dichromate was added once, and reaction 4 Add 95g of aniline and 100g of hydrochloric acid into the reaction flask, ventilate the air for 5 hours, after ventilating, add 109g of sodium carbonate, add 200 ml of saturated sodium chloride solution, and let stand to separate layers; the upper layer is viscous, and the lower layer is Water layer, separate to remove the water layer; add 200ml of ethanol to the viscous material in the upper layer, stir and let stand for half an hour, remove the upper layer, and add 50% H 2 SO 4 A total of 98g was vacuum dehydrated and dried to obtain 122g of the product. Detected by liquid chromatography, the content is 66%, and the yield is 41%.

Embodiment 3

[0016] Example 3: Add 108g of p-hydroxy-m-toluidine, 123g of N,N-dimethylaniline, 250g of hydrochloric acid, and 200g of water into a 1000ml three-neck flask, cool to about 10°C, stir, and pass air at a pressure of 0.01-0.02Mpa 6 hour, then add aniline 95g, 100g hydrochloric acid into the reaction flask, ventilate the air for 6 hours; Water layer, separate to the water layer. Add 200ml of acetone to the viscous material in the upper layer, stir and let it stand for half an hour, remove the upper layer, and add 50% H2O to the lower layer. 2 SO 4 A total of 98g was vacuum dehydrated and dried to obtain 140g of the product. Detected by liquid chromatography, the content was 86%, and the yield was 47%.

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Abstract

The invention relates to a synthesis method of a bis-(N-(7-hydroxy-8-methyl-5-phenylphenazine-3-subunit)dimethylammonium)sulfate. The method is characterized by comprising the following steps of: adding p-hydroxy-m-toluidine, N, N-dimethylaniline and hydrochloric acid into a reaction kettle, stirring them evenly, introducing air or adding sodium dichromate under a kettle pressure of 0.01-0.02Mpa, letting the materials react for 4-6h, then adding aniline and hydrochloric acid, and introducing air to make them react for 4-6h, separating the product at the end of the reaction, and subjecting the upper organic layer to neutralization, salting out, washing, acidification by sulfuric acid, dehydration as well as drying, thus obtaining the bis-(N-(7-hydroxy-8-methyl-5-phenylphenazine-3-subunit)dimethylammonium)sulfate. The synthesis method provided in the invention has the characteristics of high yield and low cost, and the prepared product has high purity.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to an acidic copper plating additive bis(N-(7-hydroxyl-8-methyl-5-phenylphenazine-3-ylidene) dimethylammonium)sulfuric acid Salt synthesis method. Background technique [0002] The structural formula of bis(N-(7-hydroxy-8-methyl-5-phenylphenazin-3-ylidene)dimethylammonium)sulfate is: , it is an acid copper copper plating brightener with excellent performance, and has excellent leveling and positioning effects. It is widely used in copper plating and alloy electroplating industry. This dye is an essential raw material for high-grade acidic copper plating brightener, and there is no literature report on this product at home and abroad. Only similar products such as saffron have been reported in the literature. However, the effect of saffron is extremely poor, and its solubility is low, so it cannot be used generally. There are similar products in foreign countries, but due ...

Claims

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Application Information

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IPC IPC(8): C07D241/46
Inventor 崔志明
Owner HUBEI LINGZHI CHEM SCI & TECH