Synthesis method of chloridized-2,3,5-triphenyl tetrazolium chloride

A technology of triphenyltetrazolium and synthesis method, applied in the direction of organic chemistry, etc., to achieve the effects of increased yield, easy source of raw materials, and high purity

Inactive Publication Date: 2014-08-13
湖北百诺捷生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second step of synthesis, the reaction is complex, and there are many negative reactions, it is necessary to strictly control the pH value of the reaction system
The above-mentioned oxidizing agents have the disadvantages of cumbersome operation and low product yield.

Method used

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  • Synthesis method of chloridized-2,3,5-triphenyl tetrazolium chloride

Examples

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Effect test

Embodiment 1

[0024] (4) Synthesis of 2,3,5-triphenyltetrazolium chloride: put the 2,3,5-triphenylformazan obtained in step (3) into a 100ml three-necked flask, and then add 60ml of methanol , turn on the stirring device, cool down to below 0°C with an ice bath, and slowly introduce Cl into the solution 2 The gas is saturated, the reaction process is obviously exothermic, and the Cl is controlled to 2 Speed, the temperature during the reaction should not exceed 15°C. With Cl 2 The feeding of the flask, the black crystals suspended in the flask gradually decreased, and the solution gradually turned brown, and when the solution was clear and free of suspended solids, stop passing Cl 2 , the reaction was stirred at room temperature for 2 h. After the reaction was completed, the solvent was evaporated under reduced pressure to obtain 6.1 g of a yellow-brown crude product with a yield of 61%. The solid was refluxed with chloroform, decolorized with activated carbon, filtered with suction, th...

Embodiment 2

[0030] (4) Synthesis of 2,3,5-triphenyltetrazolium chloride: put the 2,3,5-triphenylformazan obtained in step (3) into a 250ml three-necked flask, and then add 100ml of methanol , turn on the stirring device, cool down to below 0°C with an ice bath, and slowly introduce Cl into the solution 2 The gas is saturated, the reaction process is obviously exothermic, and the Cl is controlled to 2 Speed, the temperature during the reaction should not exceed 15°C. With Cl 2 The feeding of the flask, the black crystals suspended in the flask gradually decreased, and the solution gradually turned brown, and when the solution was clear and free of suspended solids, stop passing Cl 2 , the reaction was stirred at room temperature for 2 h. After the reaction was completed, the solvent was evaporated under reduced pressure to obtain 12.6 g of a yellow-brown crude product with a yield of 63%. The solid was refluxed with chloroform, decolorized with activated carbon, filtered with suction, ...

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Abstract

The invention discloses a synthesis method of chloridized-2,3,5-triphenyl tetrazolium chloride. The synthesis method comprises the following steps: (1) carrying out a reaction on benzaldehyde and phenylhydrazine so as to synthesize benzaldehyde-phenylhydrazone; (2) adding phenylamine into a hydrochloric acid and dripping a sodium nitrite aqueous solution at a low temperature so as to prepare a diazonium salt; (3) dripping the diazonium salt solution obtained in the step (2) into the benzaldehyde-phenylhydrazone solution obtained in the step (1) so as to synthesize 1,3,5-triphenyl formazan; and (4) dissolving the 1,3,5-triphenyl formazan obtained in the step (3) in methyl alcohol and carrying out an oxidation reaction so as to synthesize the chloridized-2,3,5-triphenyl tetrazolium chloride. The method has the characteristics that the process is simple; an oxidizing agent with high efficiency and low toxicity is adopted; the yield and the purity of the chloridized-2,3,5-triphenyl tetrazolium chloride are relatively high.

Description

Technical field: [0001] The invention relates to a method for synthesizing 2,3,5-triphenyltetrazolium chloride, which belongs to the field of chemical synthesis. Background technique: [0002] 2,3,5-triphenyltetrazolium chloride (TTC for short) has a wide range of applications in the fields of biochemistry, pharmaceutical science, medicine, agriculture, high-energy materials, automobile industry and photography. TTC is often used as analytical reagent and chromatographic analysis reagent: (1) Add an appropriate amount of TTC (0.5% TTC 1ml to 100ml agar) in the counting agar, and the bacterial colony will grow into red color, which is very meaningful for removing food background particle interference ; (2) In drug analysis - tetrazolium salt colorimetric method; Chinese Pharmacopoeia adopts triphenyl tetrazolium chloride method, such as the content determination of prednisolone acetate ointment; (3) Dehydrogenase activity determination. TTC is a redox pigment with a standa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 李清平
Owner 湖北百诺捷生物科技有限公司
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