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Method for preparing 5-phenyl-4-amino-triazolinthione

A technology of triazolethione and amino, which is applied in the field of preparation of nitrogen-containing organic corrosion inhibitors, can solve the problems of long reaction time, low synthesis yield, and many steps, and achieve shortened reaction time, optimized preparation conditions, and good application foreground effect

Inactive Publication Date: 2009-09-02
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many problems in the synthesis of 5-phenyl-4 amino-triazolethione, such as many steps, long reaction time and low synthesis yield

Method used

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  • Method for preparing 5-phenyl-4-amino-triazolinthione

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Experimental program
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Effect test

Embodiment 1

[0017] Add 0.2 mol of benzoic acid into the reaction system containing 50 ml of absolute ethanol and 8 ml of concentrated sulfuric acid, reflux at 90° C. to 100° C. for 90 minutes, and distill off unreacted ethanol. Then it was cooled to room temperature, and Na 2 CO 3 solution until the gas stops escaping, collect the organic layer, and use anhydrous CaCl 2 Dry to obtain crude ethyl benzoate. Add the obtained crude ethyl benzoate to 0.35mol 85% hydrazine hydrate and 30ml absolute ethanol, react at 90°C-100°C for 3 hours, cool to room temperature, and suction-filter the precipitated phenylhydrazide crystals. Add phenylhydrazide crystals to 50ml of absolute ethanol dissolved with 0.24mol KOH, stir and drop into 0.20mol CS 2 React at room temperature for 16 hours, add anhydrous ether and filter with suction to obtain the potassium salt. Weigh 0.05mol of the above potassium salt, add it to 0.16mol of 85% hydrazine hydrate, react at 90°C to 100°C for 4 hours, pour it into 200m...

Embodiment 2

[0019] Add 0.2 mol of benzoic acid into the reaction system containing 50 ml of absolute ethanol and 8 ml of concentrated sulfuric acid, reflux at 90° C. to 100° C. for 60 minutes, and distill off unreacted ethanol. Then it was cooled to room temperature, and Na 2 CO 3 solution until the gas stops escaping, collect the organic layer, and use anhydrous CaCl 2 Dry to obtain crude ethyl benzoate. Add the obtained crude ethyl benzoate to 0.35mol 85% hydrazine hydrate and 30ml absolute ethanol, react at 90°C to 100°C for 2.5 hours, cool to room temperature, and filter the precipitated phenylhydrazide crystals with suction. Add phenylhydrazide crystals to 50ml of absolute ethanol dissolved with 0.24mol KOH, stir and drop into 0.20mol CS 2 React at room temperature for 16 hours, add anhydrous ether and filter with suction to obtain the potassium salt. Weigh 0.05 mol of the above potassium salt, add it to 0.16 mol of 85% hydrazine hydrate, react at 90°C to 100°C for 4 hours, pour ...

Embodiment 3

[0021] Add 0.2 mol of benzoic acid into the reaction system containing 50 ml of absolute ethanol and 8 ml of concentrated sulfuric acid, reflux at 90° C. to 100° C. for 75 minutes, and distill off unreacted ethanol. Then it was cooled to room temperature, and Na 2 CO 3 solution until the gas stops escaping, collect the organic layer, and use anhydrous CaCl 2 Dry to obtain crude ethyl benzoate. Add the obtained crude ethyl benzoate to 0.35mol 85% hydrazine hydrate and 30ml absolute ethanol, react at 90°C-100°C for 3.5 hours, cool to room temperature, and suction-filter the precipitated phenylhydrazide crystals. Add phenylhydrazide crystals to 50ml of absolute ethanol dissolved with 0.50mol KOH, stir and drop into 0.20mol CS 2 React at room temperature for 16 hours, add anhydrous ether and filter with suction to obtain the potassium salt. Weigh 0.05mol of the above potassium salt, add it to 0.16mol of 85% hydrazine hydrate, react at 90°C to 100°C for 3 hours, pour into 200ml...

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Abstract

The invention discloses a method for preparing 5-phenyl-4-amino-triazolinthione, which comprises the following steps that: step one, phenylformic acid and absolute ethyl alcohol react to form ethyl benzoate; step two, the ethyl benzoate and hydrazine hydrate react to form phenylhydrazide; and step three, the phenylhydrazide and carbon bisulfide react in an absolute ethyl alcohol solution of potassium hydroxide to form potassium salt, and then the potassium salt and the hydrazine hydrate react to form the 5-phenyl-4-amino-triazolinthione. The method ensures that the reaction time is greatly shortened by optimizing preparation conditions; and the method has good application prospect.

Description

technical field [0001] The invention relates to a preparation method of a nitrogen-containing organic corrosion inhibitor, which belongs to the field of acid corrosion inhibitors. Background technique [0002] The problem of metal corrosion pervades all areas of the national economy. Although it is inevitable, it can be prevented and slowed down. At present, the anti-corrosion technology of metal mainly includes the application of corrosion-resistant materials, surface anti-corrosion technology, addition of corrosion inhibitors and electrochemical protection. Among them, the method of adding corrosion inhibitor is a simple, cheap and applicable anti-corrosion method. [0003] Among the many corrosion inhibitors, most practical corrosion inhibitors are compounds composed of active group molecules containing N, O, S, P and other atoms or unsaturated bonds that are easy to provide lone pairs of electrons. Among nitrogen-containing compound corrosion inhibitors, Mannich bases,...

Claims

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Application Information

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IPC IPC(8): C07D249/12
Inventor 冯辉霞张茵赵丹魏云张义新赵霞张婷王毅
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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