Preparation method of 2,3,5-triphenyltetrazolium chloride

A technology of triphenyl tetrazolium chloride and triphenyl formazan, which is applied in the field of preparation of phenyl tetrazolium chloride, can solve the problems of human harm and environmental pollution, and achieve the effect of improving product quality

Inactive Publication Date: 2018-11-30
湖南恒泰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The lead tetraacetate used in this method is a heavy metal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 212 g (2 mol) of freshly distilled benzaldehyde were dissolved in 1250 ml of methanol, and 216 g (2 mol) of phenylhydrazine were added with stirring. In the process of adding phenylhydrazine, there is a small amount of heat release, so the temperature should not exceed 30°C; the obtained product should be sealed and stored away from light;

[0026] Add 200 grams of sodium hydroxide and 200 grams of anhydrous sodium acetate to 2L of methanol for stirring and dissolving, and when the temperature is lowered to 0°C, add 150 grams of benzaldehyde phenylhydrazone and stir the liquid evenly; another 186 grams of aniline (2mol), 500ml of concentrated hydrochloric acid, 200ml of water is made into aniline hydrochloride solution, the liquid is cooled to 0°C, and 250ml of water and 140-150 grams of sodium nitrite are made into a solution.

[0027] Slowly add the diazonium salt into the solution prepared in the second step under stirring, control the reaction temperature not to exc...

Embodiment 2

[0030] 1060 g (5 mol) of freshly distilled benzaldehyde was dissolved in 3125 ml of methanol, and 540 g (5 mol) of phenylhydrazine was added under stirring. In the process of adding phenylhydrazine, there is a small amount of heat release, so the temperature should not exceed 30°C; the obtained product should be sealed and stored away from light;

[0031] Add 500 grams of sodium hydroxide and 500 grams of anhydrous sodium acetate to 5 L of methanol to stir and dissolve, and when the temperature is lowered to 0 ° C, add 375 grams of benzaldehyde phenylhydrazone and stir the liquid evenly; another 465 grams of aniline (5mol), 2500ml of concentrated hydrochloric acid, 500ml of water is made into aniline hydrochloride solution, the liquid is cooled to 0°C, 625ml of water and 350-375 grams of sodium nitrite are made into a solution.

[0032] Slowly add the diazonium salt into the solution prepared in the second step under stirring, control the reaction temperature not to exceed 5°C...

Embodiment 3

[0035] Dissolve 42.4 kg (400 mol) of freshly distilled benzaldehyde in 250 L of methanol, and add 43.2 kg (400 mol) of phenylhydrazine under stirring. In the process of adding phenylhydrazine, there is a small amount of heat release, so the temperature should not exceed 30°C; the obtained product should be sealed and stored away from light;

[0036] Add 40 kg of methanol to 40 kg of sodium hydroxide and 40 kg of anhydrous sodium acetate for stirring and dissolving, and when cooling to 0°C, add 300 kg of benzaldehyde phenylhydrazone and stir the liquid evenly; in addition, 37.2 kg of aniline (400mol), 1001 concentrated hydrochloric acid, 4001 water is made into aniline hydrochloride solution, the liquid is cooled to 0°C, 5001 water and 28-30 kg of sodium nitrite are made into a solution.

[0037] Slowly add the diazonium salt into the solution prepared in the second step under stirring, control the reaction temperature not to exceed 5°C, and precipitate red small crystals, stir...

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PUM

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Abstract

The invention relates to phenyltetrazolium chloride, and in particular, relates to a preparation method of phenyltetrazolium chloride. The preparation method comprises the steps: with benzaldehyde, aniline and phenylhydrazine as basic raw materials, synthesizing phenylhydrazone by benzaldehyde and phenylhydrazine firstly, then synthesizing triphenylformazan red crystals from diazonium salt formedby aniline, and then cyclizing into 2,3,5-triphenyltetrazolium chloride by using an organic catalyst. The process completely avoids use of lead tetraacetate as the catalyst to synthesize the product.Compared with a traditional process, the preparation method does not use lead tetraacetate, eliminates the influence of lead on the environment, and has the yield reaching 70% or more and the purity of more than or equal to 99% (HPLC).

Description

technical field [0001] The invention relates to phenyl tetrazolium chloride, in particular to a preparation method of phenyl tetrazolium chloride. Background technique [0002] 2,3,5-Triphenyltetrazolium chloride is a sensitive reagent for reducing sugars, it can distinguish ethanol, ketones and simple aldehydes. Determination of dehydrogenase activity. Titration of diborane, pentaborane and decaborane It can also be used to test the germination rate of plant seeds, determine the activity of dehydrogenase, titrate borane, and analyze the residual amount of pesticides; it can be seen that this is an important reagent. [0003] The usual process is the synthesis method on page 841 of "Organic Synthesis Codex": dissolve triphenylformazan in chloroform, add lead tetraacetate under freezing conditions until the red color disappears. Chloroform was evaporated, the residue was dissolved in water, hydrochloric acid was added, and lead chloride was precipitated. Filter and extract ...

Claims

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Application Information

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IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 伍雄飞张复兴许志锋伍雄姿伍建军谭斌刘明明朱小明盛良兵彭卫红
Owner 湖南恒泰化工有限公司
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