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Synthesis of electronic chemical 5-amino tetrazole

A technology of aminotetrazole and electronic chemicals, applied in organic chemistry and other directions, can solve problems such as danger and easy explosion, and achieve the effect of high product yield and simple process

Inactive Publication Date: 2012-01-18
NANTONG HUAFENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The existing production of 5-aminotetrazole is obtained by cyclization of dicyandiamide as the starting material and sodium azide. The use of sodium azide in the process is dangerous and prone to explosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 81 grams of hydrazine hydrate to a 1000 ml three-necked flask, slowly add 39 grams of sulfuric acid under stirring, and start to drop it quickly to make the temperature reach 40 ° C, control the temperature between 28-32 ° C, and add 30% cyanamide 180 Grams were added rapidly. After all the additions were complete, the temperature was raised to 60°C and kept constant 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 add the sodium nitrite solution prepared by 82.8 grams of sodium nitrite and 238 grams of water dropwise in about 1.5 hours. 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 100 ml of water, heat up to 85°C, maintain the temperature between 85°C-88°C for 3 hours, and cool At 10°C, the obtained solid was filtered to obtain a...

Embodiment 2

[0013] Add 81 grams of hydrazine hydrate into a 1000 ml three-necked flask, slowly add 78.9 grams of concentrated hydrochloric acid under stirring, and start to drop quickly to make the temperature reach 40°C, and control the temperature between 28-32°C to dissolve 30% cyanamide 180 grams were added rapidly. After all the additions were complete, 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, add 82.8 grams of sodium nitrite and 238 grams of water to the sodium nitrite solution dropwise in about 1.5 hours. above reaction solution. Control the reaction solution at a constant temperature between 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 85°C-88°C for 3 hours, and cool At 10°C, the obtained solid was filtered to obtai...

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PUM

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Abstract

The invention discloses a synthesis and production method of an electronic chemical 5-amino tetrazole. The method comprises the following steps of: firstly carrying out neutralization reaction on hydrazine hydrate and acid, then adding a cyanamide aqueous solution, reacting to generate aminoguanidine salt, carrying out diazotization with sodium nitrite under acidic conditions to obtain ether azide, carrying out ring-closure reaction under alkaline conditions to obtain a crude product of the 5-amino tetrazole, and refining with water to obtain a qualified product. The method disclosed by the invention has simple process and high product yield, and is easy to operate.

Description

technical field [0001] The invention relates to the synthesis of electronic chemical 5-aminotetrazole. Background technique [0002] The existing production of 5-aminotetrazole is obtained by reacting dicyandiamide with sodium azide as the starting material, and sodium azide used in the process is dangerous and prone to explosion. Contents of the invention [0003] The purpose of the invention is to provide a production method of 5-aminotetrazole with simple process, safe and reliable, and high yield. [0004] Technical solution of the present invention is: [0005] Neutralize with hydrazine hydrate and acid first, then add cyanamide aqueous solution to generate aminoguanidine salt, diazotize with sodium nitrite under acidic conditions to obtain azide, and close the ring under alkaline conditions to obtain 5-aminotetrazolium The crude product is purified by water to obtain the qualified product 5-aminotetrazole, the reaction formula is: [0006] [0007] The molar ra...

Claims

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Application Information

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IPC IPC(8): C07D257/06
Inventor 王德峰张耀斌王炳才朱小飞俞健钧
Owner NANTONG HUAFENG CHEM