Chemical synthesis method of 1,2,3,4-tetra nitroazole kind compound

A technology of chemical synthesis and tetrazole, which is applied in the field of 1, can solve the problems of high reaction temperature and low yield, and achieve the effects of high reaction yield, low dosage and low production cost

Inactive Publication Date: 2006-01-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method requires an equimolar amine salt as a catalyst,...

Method used

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  • Chemical synthesis method of 1,2,3,4-tetra nitroazole kind compound
  • Chemical synthesis method of 1,2,3,4-tetra nitroazole kind compound
  • Chemical synthesis method of 1,2,3,4-tetra nitroazole kind compound

Examples

Experimental program
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Embodiment 1

[0034] The molar ratio of nitrile, sodium azide, and zinc trifluoromethanesulfonate is 1:1:0.1, the nitrile is benzonitrile, and the water consumption is 10 times of the nitrile mass.

[0035] In a 150ml four-necked flask equipped with a thermometer, reflux condenser and mechanical stirring, add 100g of water, 10.3g (0.1mol) of benzonitrile, 6.5g (0.1mol) of sodium azide, and 3.63g of zinc trifluoromethanesulfonate (10mmol), heated to reflux (100°C), and refluxed for 4 hours. After the reaction was completed, it was cooled to room temperature and neutralized to pH=5 with concentrated hydrochloric acid. Filter and collect the precipitated white solid to obtain 13.4 g of 5-phenyl-1H-tetrazolium with a yield of 90%, a purity of 98.2%, and a melting point of 215°C.

Embodiment 2

[0037] The molar ratio of nitrile, sodium azide and zinc trifluoromethanesulfonate is 1:1:1, the nitrile is benzonitrile, and the water consumption is 10 times of the nitrile mass. 10.3 g (0.1 mol) of benzonitrile, 6.5 g (0.1 mol) of sodium azide, 36.3 g (0.1 mol) of zinc trifluoromethanesulfonate, and the reaction temperature was 90°C.

[0038] Others were the same as in Example 1 to obtain 14.1 g of 5-phenyl-1H-tetrazolium with a yield of 95%, a purity of 98.3%, and a melting point of 215°C.

Embodiment 3

[0040] The molar ratio of nitrile, sodium azide and zinc trifluoromethanesulfonate is 1:1:0.5, the nitrile is benzonitrile, and the water consumption is 30 times of the nitrile mass. 10.3 g (0.1 mol) of benzonitrile, 6.5 g (0.1 mol) of sodium azide, 18.2 g (50 mmol) of zinc trifluoromethanesulfonate, and the reaction time was 6 hours.

[0041] Others were the same as in Example 1 to obtain 13.8 g of 5-phenyl-1H-tetrazolium with a yield of 93%, a purity of 98.5%, and a melting point of 215°C.

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Abstract

A process for chemically synthesizing 1, 2, 3, 4-tetrazolium includes such steps as dissolving zinc trifluoro methylsulfonate in water, adding nitrile and sodium azide, reacting, adding acid for neutralizing and filter. Its advantages are high output rate, and no pollution.

Description

(1) Technical field [0001] The invention relates to a chemical synthesis method of 1,2,3,4-tetrazolium compounds. (2) Background technology [0002] 1,2,3,4-tetrazolium compounds are widely used in the synthesis of pesticides, medicines and dyes, and have high practical value. [0003] In the prior art, the chemical synthesis of 1,2,3,4-tetrazolium compounds is prepared in an organic solvent with an amine or amine salt catalyst. As proposed in US 4,097,479, it is prepared by reacting 1 mol of nitrile and 1 mol of sodium azide under the catalysis of 1 mol of amine salt. This method requires an equimolar amine salt as a catalyst, the reaction temperature is higher, and the yield is generally lower. (3) Contents of the invention [0004] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a 1,2,3,4-tetrazolium with reasonable process, high reaction yield, less catalyst consumption, convenient recovery and mechanical application,...

Claims

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Application Information

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IPC IPC(8): C07D257/04
Inventor 苏为科金灿
Owner ZHEJIANG UNIV OF TECH
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