Method for one-pot synthesis of 2,6-diaminopyrazine-1-oxide
A technology of diaminopyrazine and oxide, which is applied in the direction of organic chemistry, and can solve problems such as severe conditions, unsuitable for industrial production, and excessive production of three wastes
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Embodiment 1
[0034] This embodiment provides the preparation method of 2,6-diaminopyrazine-1-oxide of the present invention, specifically:
[0035] At 5°C, add 19.02Kg (200mol) of iminodiacetonitrile into a 100L titanium alloy pressure reactor, then add 10mol of acidic catalyst concentrated nitric acid, solvent methanol 60L, and feed nitrogen monoxide 9.03Kg (300mol) under a pressure of 20MPa. Keep stirring at 5°C for sufficient reaction for 5 hours; then control the temperature of the reaction solution to less than 15°C, add 22.9Kg (400mol) hydroxylamine in batches, stir and react at 5°C for 4 hours, then stir and react at 25°C for 8 hours, filter, and filter the cake through After washing with methanol and drying, 22.23 Kg of off-white solid 2,6-diaminopyrazine-1-oxide was obtained, with a yield of 88.7% and a purity of 99.8%.
[0036] The melting point of the 2,6-diaminopyrazine-1-oxide prepared in this example is 294.1°C-294.9°C, and its TGA / DSC spectrum is as attached figure 1 shown....
Embodiment 2
[0042] This embodiment provides the preparation method of 2,6-diaminopyrazine-1-oxide of the present invention, specifically:
[0043]At 35°C, add 19.02Kg (200mol) of iminodiacetonitrile into a 100L titanium alloy pressure reactor, then add 11mol 7mol / l sulfuric acid, solvent DMF 50L, and feed 7.8Kg (260mol) of nitric oxide under a pressure of 10MPa. Stir and react at 35°C for 3 hours; then control the temperature of the reaction solution to less than 15°C and add hydroxylamine (300mol) in batches, stir and react at 1°C for 3h, then stir and react at 20°C for 5h, evaporate the solvent under reduced pressure to obtain a brown solid , the filter cake was stirred with methanol, washed, filtered, and dried to obtain 20.3Kg of 2,6-diaminopyrazine-1-oxide, with a yield of 80.5% and a purity of 98.1%.
Embodiment 3
[0045] 0°C, add 1.902Kg (20mol) of iminodiacetonitrile into the 10L titanium alloy pressure reactor, then add 1mol7mol / l catalyst sulfuric acid, solvent ethanol 5L, feed nitrogen monoxide 0.60Kg (20mol) under 1MPa pressure, in Stir and react at 0°C for 2 hours; then control the temperature of the reaction solution to less than 15°C, add 0.73Kg (22mol) of hydroxylamine in batches, stir and react at 0°C for 2h, then stir and react at 25°C for 5h, evaporate the solvent under reduced pressure, A brown solid was obtained, and the filter cake was stirred with ethanol, washed, filtered, and dried to obtain 1.95 Kg of 2,6-diaminopyrazine-1-oxide, with a yield of 77.3% and a purity of 99%.
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Abstract
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