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Method for catalytic synthesis of 5-substituted tetrazole by tungstate

A technology of tungstate and tetrazole, which is applied in the field of synthesis of 5-substituted tetrazole, can solve the problems of difficult catalyst recovery, high cost, unsuitable for industrial production, etc., and achieve the effect of easy separation, easy operation and high activity

Inactive Publication Date: 2010-02-24
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods will produce highly toxic and explosive azide, which is not suitable for industrial production
On the other hand, catalyst recovery is difficult and the cost is too high

Method used

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  • Method for catalytic synthesis of 5-substituted tetrazole by tungstate
  • Method for catalytic synthesis of 5-substituted tetrazole by tungstate
  • Method for catalytic synthesis of 5-substituted tetrazole by tungstate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 2.5 mmol benzonitrile in 5 ml DMF, add 2.6 mmol sodium azide, 0.23 mmol barium tungstate (BaWO 4 ), reacted at 120 degrees centigrade for 24 hours, centrifuged the reaction solution after cooling, filtered out the catalyst, neutralized the filtrate with 6mol / L hydrochloric acid, extracted with ethyl acetate and rotary evaporated the organic layer to obtain a solid product with a yield of 75%.

Embodiment 2

[0020] Dissolve 2.5 mmol benzonitrile in 5 ml DMF, add 2.6 mmol sodium azide, 0.80 mmol barium tungstate (BaWO 4 ), reacted at 120 degrees centigrade for 24 hours, centrifuged the reaction solution after cooling, filtered the catalyst, neutralized the filtrate with 6mol / L hydrochloric acid, extracted with ethyl acetate and rotary evaporated the organic layer to obtain a solid product with a yield of 75%.

Embodiment 3

[0022] Dissolve 2.5 mmol benzonitrile in 5 ml DMF, add 5.4 mmol sodium azide, 0.80 mmol barium tungstate (BaWO 4 ), reacted at 120 degrees centigrade for 24 hours, centrifuged the reaction solution after cooling, filtered the catalyst, neutralized the filtrate with 6mol / L hydrochloric acid, extracted with ethyl acetate and rotary evaporated the organic layer to obtain a solid product with a yield of 75%.

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Abstract

The invention discloses a method for synthesizing 5-substituted tetrazolium through tungstate catalysis. Firstly, nitrile and sodium azide are dissolved in an organic solvent according to 1: 1.05-2.1mol ratio, then the nitrile with 1 / 10 to 1 / 3 mol ratio is added into a tungstate catalyst for reaction for 12 to 24 hours at 120 DEG C; after the obtained reaction liquid is cooled, insoluble substances are removed through centrifugation or filtering, and 6 mol / L hydrochloric acid is added into the filter liquor for neutralization; the filter liquor after being neutralized is extracted by using ethyl acetate, and an organic layer is rotated and evaporated to obtain the product. In the invention, tungstate is used as the catalyst, and in the organic solvent, through the two-phase reaction between the nitrile and the sodium azide, 5-substituted tetrazolium is obtained. The adopted tungstate catalyst has the advantages of high activity, easy separation, and periodic application. The process of the method is simple, the operation is easy, the catalyst can be recovered to be used, and the yield rate of the product can reach 75 to 97 percent.

Description

technical field [0001] The invention relates to a method for synthesizing 5-substituted tetrazole, in particular to a method for catalytically synthesizing 5-substituted tetrazole with tungstate. Background technique [0002] 5-substituted tetrazoles are widely used in many fields such as medicine, pesticide and fine chemical industry. The traditional method for synthesizing tetrazole is mainly to prepare by reacting nitrile and azide in solution under the action of catalyst, or by reacting nitrile and sodium azide under the action of solvent and ammonium salt. Above methods all can produce highly toxic and explosive azide, which is unsuitable for suitability for industrialized production. On the other hand, catalyst recovery is difficult and the cost is too high. Invention content: [0003] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a method for synthesizing 5-substituted tetrazoles that is sa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/04B01J23/30B01J23/888
CPCY02P20/584
Inventor 徐正贺竞辉李保军
Owner NANJING UNIV