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Preparation method of tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine

A technology based on oxides and pyridyl, which is applied in the field of preparation of tris[2-ethyl]amine, can solve the problems of difficulty, loss, and easy pollution, etc., so as to improve product yield, increase electrophilicity, Effects of strong nucleophilicity and reactivity

Inactive Publication Date: 2017-05-17
江苏燎原环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both raw materials need to be recycled during post-processing, which is difficult, wasteful, and easy to cause pollution

Method used

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  • Preparation method of tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine
  • Preparation method of tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine
  • Preparation method of tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 250ml four-necked reaction flask, add 50ml of anhydrous methanol and 0.055mol of sodium methoxide to obtain a sodium alkoxide solution, add 0.05mol of newly prepared tris(2-mercaptoethyl)amine, react for 20 minutes, and add newly prepared 2-chloropyridine-N-oxide 0.15mol. Heating to reflux, TLC tracking the whole process of the reaction, and timely qualitative and quantitative determination of the product and the end of the reaction, to stop the reaction. After cooling, filter and recover low boilers under reduced pressure on a rotary evaporator. Add an aqueous solution containing hydrochloric acid to the high boiling residue and stir evenly, adjust the pH to 3, extract three times with ethyl acetate, dry the organic phase with anhydrous sodium sulfate, remove the solvent under reduced pressure on a rotary evaporator to obtain a light yellow liquid crude product, crude The product was purified by column chromatography, and the solvent was recovered from the eluent...

Embodiment 2

[0035] In a 250ml four-necked reaction flask, add 40ml of anhydrous methanol and 0.045mol potassium ethylate to obtain a potassium alcoholate solution, add newly prepared tris(2-mercaptoethyl)amine (0.03mol) and react for 15 minutes, then add dropwise 0.112 mol of 2-chloropyridine-N-oxide, other preparation processes are the same as in Example 1, and the resulting product yield is 80.8%.

Embodiment 3

[0037]In a 250ml four-necked reaction flask, add 60ml of anhydrous methanol and 0.065mol potassium ethylate to obtain a potassium alcoholate solution. After adding newly prepared tris(2-mercaptoethyl)amine (0.08mol) to react for 25 minutes, add dropwise 0.175 mol of 2-chloropyridine-N-oxide, other preparation processes are the same as in Example 1, and the resulting product yield is 82.5%.

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Abstract

The invention discloses a preparation method of tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine, namely taking a path for synthesizing the tri[2-(N-oxide-pyridine-2-sulfenyl)ethyl]amine through the interaction of 2-chloropyridine-N-oxide and tri(2-mercapto ethyl)amine. The oxygen on the N- reinforces the electrophilicity of alpha-position carbon on a pyridine ring, the alkaline media reinforces nucleophilicity of mercaptan negative ion, the reactivity of two reactant is sufficiently utilized, the cheap and excess 2-chloropyridine-N-oxide can be recycled, so that the preparation method disclosed by the invention is high in yield and less in material consumption.

Description

technical field [0001] The invention belongs to the technical field of marine antifouling, and specifically relates to a preparation method of tris[2-(N-oxide-pyridyl-2-thio)ethyl]amine, which is mainly used for producing antifouling in marine antifouling coatings. Pollution agent to prevent marine organisms from attaching and growing on the surface of marine facilities such as breeding nets, ships, offshore oil and gas platforms, piers, bridge piers, and seawater pipelines. Background technique [0002] The attachment and growth of marine organisms on the surface of marine facilities is called marine biofouling. Marine biofouling can increase the navigation resistance of ships, block pipelines and breeding nets, affect the normal use of acoustic instruments and other offshore equipment, and increase offshore oil pollution. And the burden of natural gas exploitation platform, accelerated metal corrosion and other serious hazards, resulting in huge losses in marine military a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 崔健栾和林储正相冯启明
Owner 江苏燎原环保科技股份有限公司
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