A kind of trinitromethylazole energetic compound and preparation method thereof
A technology of trinitromethylazoles and trinitromethyl, which is applied in the field of trinitromethylazole energetic compounds and their preparation, can solve the problems of obtaining products without separation, and achieve easy separation and reaction conditions mild effect
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Embodiment 1
[0036]Under a low-temperature bath at -15°C, 1.1g (7.7mmol) of 5-amino-1,2,4-triazole-3-carboxylic acid and 0.35g (1.6mmol) of bis(5-nitroamine-1,2 ,4-triazole)ethane hydrochloride was successively added to 8mL of fuming nitric acid, and the addition temperature should not exceed 0°C. After all the raw materials were dissolved, 12 mL of concentrated sulfuric acid was slowly added dropwise at -10°C. After the addition of concentrated sulfuric acid, stirring was continued at -5°C for 0.5 h, and then returned to 20°C for 12 h. Pour the reaction solution into 100g of crushed ice to quench, filter out the by-product bis(5-nitroamine-1,2,4-triazole)ethane, extract the filtrate 10 times with 50mL dichloromethane, and extract the organic The phase was dried with anhydrous magnesium sulfate and then spin-dried at room temperature to obtain 0.84 g of a light yellow solid with a yield of 44.9%.
Embodiment 2
[0038] Under a low-temperature bath at -15°C, 1.1g (7.7mmol) of 5-amino-1,2,4-triazole-3-carboxylic acid and 0.7g (3.2mmol) of bis(5-nitroamine-1,2 ,4-triazole)ethane hydrochloride was successively added to 8mL of fuming nitric acid, and the addition temperature should not exceed 0°C. After all the raw materials were dissolved, 12 mL of concentrated sulfuric acid was slowly added dropwise at -5°C. After the addition of concentrated sulfuric acid, the mixture was stirred at -5°C for 0.5h, and then returned to 22°C for 12h. Pour the reaction solution into 100g of crushed ice to quench, filter out the by-product bis(5-nitroamine-1,2,4-triazole)ethane, extract the filtrate 10 times with 80mL dichloromethane, and extract the organic The phase was dried with anhydrous magnesium sulfate and then spin-dried at room temperature to obtain 1.58 g of light yellow solid with a yield of 88.7%.
Embodiment 3
[0040] Under a low-temperature bath at -15°C, 1.1g (7.7mmol) of 5-amino-1,2,4-triazole-3-carboxylic acid and 1.04g (4.8mmol) of bis(5-nitroamine-1,2 ,4-triazole)ethane hydrochloride was successively added to 8mL of fuming nitric acid, and the addition temperature should not exceed 0°C. After all the raw materials were dissolved, 12mL of concentrated sulfuric acid was slowly added dropwise at 0°C. After the addition of concentrated sulfuric acid, the mixture was stirred at 5°C for 0.5h, and then returned to 25°C for 12h. Pour the reaction solution into 100g of crushed ice to quench, filter out the by-product bis(5-nitroamine-1,2,4-triazole)ethane, extract the filtrate 10 times with 100mL dichloromethane, and extract the organic The phase was dried with anhydrous magnesium sulfate and then spin-dried at room temperature to obtain 1.26 g of light yellow solid with a yield of 67.4%.
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