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Method for preparing triphenyltetrazolium chloride

A technology for chlorinating triphenyltetrazolium and phenol, which is applied in the field of preparation of triphenyltetrazolium chloride, can solve the problems of high production cost, short reaction time, complicated technological process and the like, and achieves low production cost, The effect of reducing waste water discharge and simple process

Inactive Publication Date: 2016-10-26
SUQIAN YUANYANG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for preparing phenyltetrazolium has the characteristics of complex process flow, various operation steps, and large loss of organic solvent, which is not conducive to industrial production
[0003] In response to the above phenomenon, Chinese Patent No. 231813297884.7 proposes a preparation method of phenyltetrazolium, using N,N-dimethylformamide as a reaction solvent, benzonitrile as a raw material, and sodium azide and ammonium chloride The crude product of phenyltetrazolium is prepared by reaction, then added with absolute ethanol for refining, centrifuged and dried to obtain the finished product of phenyltetrazolium; the method has a short reaction time, which is beneficial to reduce energy consumption, increase production batches, and improve Yield; the design of the refining process is conducive to improving the purity of the product, and at the same time the refined solvent ethanol can be recycled; but the reactants used in this method are relatively large, which makes the production cost higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation method of triphenyl tetrazolium chloride, comprising the following steps:

[0018] (1) Synthesis of benzaldehyde: Add phenol into the reaction vessel, dissolve it in an organic solvent, then add methanol, heat and stir, and control the heating temperature at 38°C. After the phenol is completely dissolved, stop heating, and cool to 8°C while stirring. Adding toluene reacts slightly exothermic, and precipitates milky white needle-like precipitates, continues to stir for 2h, stands still for 1h, and filters the reaction solution to obtain milky white needle-like solids, which are benzaldehyde. The organic solution is dimethyl sulfoxide, hexane With the mixed solution of dichloromethane, its molar ratio is 2:2:1;

[0019] (2) Synthesis of diazonium salt: Add hydrochloric acid and aniline into the reaction vessel, cool to 8°C, then slowly add a slightly excessive amount of 233% sodium nitrite solution dropwise, the reaction solution continues to stir for 123 mi...

Embodiment 2

[0022] A preparation method of triphenyl tetrazolium chloride, comprising the following steps:

[0023] (1) Synthesis of benzaldehyde: Add phenol into the reaction vessel, dissolve it in an organic solvent, then add methanol, heat and stir, and control the heating temperature at 38°C. After the phenol is completely dissolved, stop heating, and cool to 8°C while stirring. Adding toluene reacts slightly exothermic, and precipitates milky white needle-like precipitates, continues to stir for 2h, stands still for 1h, and filters the reaction solution to obtain milky white needle-like solids, which are benzaldehyde. The organic solution is dimethyl sulfoxide, hexane With the mixed solution of dichloromethane, its molar ratio is 2:2:1;

[0024] (2) Synthesis of diazonium salt: Add hydrochloric acid and aniline into the reaction vessel, cool to 3°C, then slowly add a slightly excessive amount of 233% sodium nitrite solution dropwise, the reaction solution continues to stir for 123 mi...

Embodiment 3

[0027] A preparation method of triphenyl tetrazolium chloride, comprising the following steps:

[0028] (1) Synthesis of benzaldehyde: Add phenol into the reaction vessel, dissolve it in an organic solvent, add methanol, heat and stir, and control the heating temperature at 43°C. After the phenol is completely dissolved, stop heating and cool to 8°C while stirring. Adding toluene reacts slightly exothermic, and precipitates milky white needle-like precipitates, continues to stir for 2h, stands still for 1h, and filters the reaction solution to obtain milky white needle-like solids, which are benzaldehyde. The organic solution is dimethyl sulfoxide, hexane With the mixed solution of dichloromethane, its molar ratio is 2:2:1;

[0029] (2) Synthesis of diazonium salt: Add hydrochloric acid and aniline into the reaction vessel, cool to 4°C, then slowly add a slightly excessive amount of 233% sodium nitrite solution dropwise, the reaction solution continues to stir for 123 minutes,...

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Abstract

The invention discloses a method for preparing triphenyltetrazolium chloride. The method comprises the following steps: (1) synthesizing benzaldehyde; (2) synthesizing a diazonium salt; (3) synthesizing triphenyltetrazolium chloride. The method for preparing the triphenyltetrazolium chloride has the advantages that the process is simple, safe and easy to operate, and a catalyst used in the reaction process can be recycled, and thus the production cost is low; the synthesis method is environment-friendly, and is suitable for industrial production, and the wastewater discharge is greatly reduced; meanwhile, the product synthesized by the method has a yield of up to 88%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of triphenyltetrazolium chloride. Background technique [0002] At present, almost all manufacturers at home and abroad use organic solvents such as ethyl acetate, DMF, and DMSO as reaction system solvents, and through complex processes such as multiple extractions, distillations, and separations under the action of phase transfer catalysts, phenyltetrazolium is produced. Salt, then acidified to obtain crude phenyl tetrazole, refined to obtain fine phenyl tetrazole. The existing method for preparing phenyltetrazolium has the characteristics of complex process flow, numerous operation steps, and large loss of organic solvent, which is unfavorable for industrial production. [0003] In response to the above phenomenon, Chinese Patent No. 231813297884.7 proposes a preparation method of phenyltetrazolium, using N,N-dimethylformamide as a reaction solve...

Claims

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Application Information

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IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 袁雪生张宏杰
Owner SUQIAN YUANYANG BIOTECH
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