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A kind of new synthetic method of 5-phenyltetrazolium

A phenyltetrazolium, a newly synthesized technology, applied in the direction of organic chemistry, can solve the problems of explosion and danger, and achieve the effect of high product yield and simple synthesis process

Inactive Publication Date: 2015-10-21
姜树林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing production of 5-phenyltetrazolium is obtained by cyclization reaction of benzonitrile as starting material and sodium azide in different solvents. The use of sodium azide in the process is dangerous and prone to explosion

Method used

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  • A kind of new synthetic method of 5-phenyltetrazolium

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Embodiment 1

[0013] Add 81 grams of hydrazine hydrate into the three-necked flask, slowly add 39 grams of sulfuric acid under stirring, and start the rapid dropwise addition to make the temperature reach 40°C, control the temperature between 28 and 32°C, mix 130 grams of benzonitrile, 150 ml of water The solution prepared with 150 milliliters of ethanol was added rapidly, and after all the additions were completed, the temperature was raised to 60° C., and kept at this temperature for 3 hours. After cooling to about 35°C, add 200 grams of reagent hydrochloric acid, control the reaction temperature at 10-15°C, and dropwise add sodium nitrite solution prepared by 81 grams of sodium nitrite and 238 grams of water to the above reaction solution. Control the reaction solution at a constant temperature between 20-25°C for 18 hours, add a solution prepared by adding 90 grams of sodium hydroxide and 110 ml of water, heat up to 85°C, and keep the temperature between 85°C-88°C for 3 hours. Cool to ...

Embodiment 2

[0015] Add 81 grams of hydrazine hydrate into the three-necked flask, slowly add 78.9 grams of concentrated hydrochloric acid under stirring, and start to add it dropwise quickly, so that the temperature reaches 40 ° C, and control the temperature between 28 and 32 ° C. Mix 130 grams of benzonitrile and 150 ml of water The solution prepared with 150 milliliters of ethanol was added, and after all the additions were completed, the temperature was raised to 60° C., and kept at this temperature for 3 hours. After cooling to about 35°C, add 128 grams of reagent hydrochloric acid, control the reaction temperature at 10-15°C, and add the sodium nitrite solution prepared by 81.2 grams of sodium nitrite and 238 grams of water dropwise in about 1.5 hours. above reaction solution. Control the temperature of the reaction solution at 20-25°C for 18 hours, add a solution prepared by adding 48.5 grams of sodium hydroxide and 100 ml of water, heat up to 85°C, maintain the temperature between...

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Abstract

The invention discloses a novel synthetic method for 5-phenyl tetrazole, which includes the following steps: firstly performing acid neutralization to hydrazine hydrate; then adding mixing solution formed by cyanobenzene, water and ethyl alcohol to generate phenyl aminoguanidine salt; adopting sodium nitrite for diazotization to obtain nitrine amidine under the acidic condition; obtaining 5-phenyl tetrazole crude product through closed loop under the alkaline condition; obtaining 5-phenyl tetrazole acceptable product through adopting ethyl alcohol for refining. The method has the advantages of simple technology, simplicity in operation and high product yield.

Description

technical field [0001] The invention relates to a method for synthesizing 5-phenyltetrazolium, a key intermediate of sartan drugs. Background technique [0002] 5-Phenyltetrazolium is a white crystalline powder with a melting point of 209-212°C and a molecular formula of C 7 h 6 N 4 , mainly used in the synthesis of a new generation of cephalosporin antibiotics, and its intermediates have a wide range of uses in the synthesis of antifungal drugs. The existing production of 5-phenyltetrazolium is obtained by cyclization reaction of benzonitrile as starting material and sodium azide in different solvents. The use of sodium azide in the process is dangerous and prone to explosion. Contents of the invention [0003] The object of the present invention is to aim at the deficiencies in the prior art, to provide a kind of process simple, safe and reliable, the production method of the 5-phenyltetrazolium of high yield. [0004] In order to solve the above technical problems, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/04
Inventor 王德峰张耀斌王炳才吴迪山朱小飞俞建钧
Owner 姜树林