The preparation method of acetonitrile
A technology of acetonitrile and concentrated nitric acid, which is applied in the preparation of organic compounds, the preparation of urea derivatives, the preparation of amino compounds, etc., can solve the problems of harsh hydrolysis conditions, low yield, complicated reaction operation steps, etc., and achieves improved yield , the effect of simplifying the synthesis process
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Embodiment 1
[0017] Dissolve 132g of N,N'-diethylurea in 200mL of dichloromethane to prepare a solution, slowly add it to 278g of concentrated nitric acid with a mass concentration of 98% and 233g of 20% oleum to form a mixed acid for nitration reaction, the reaction temperature -5°C to 0°C. After the addition, the reaction mixture was poured into 400 g of ice water for dilution.
[0018] The dilute solution was heated to 20°C for hydrolysis reaction. The hydrolysis time was 60 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, the dichloromethane phase was dried with anhydrous magnesium sulfate, and concentrated to obtain 165 g of dinitroamine with a yield of 80.6%. ≥99.3%.
[0019] Structural identification of dinitramine:
[0020] Elemental Analysis: C 2 h 6 N 2 o 2 , calculated: C 26.67, H 6.667, N 31.11;
[0021] Found: C 27.01, H 6.593, N 30.82.
[0022] IR(KBr),υ / cm -1 : 2978, 2879, 1532, 1381, 778.
[0023] 1 H NMR (CDCl 3 ,δ,ppm):1.01...
Embodiment 2
[0026] Dissolve 132g of N,N'-diethylurea in 200mL of dichloromethane to prepare a solution, slowly add 201g of concentrated nitric acid with a mass concentration of 98% and 169g of 20% oleum to form a mixed acid for nitration reaction, the reaction temperature -5°C to 0°C. After the addition, the reaction mixture was poured into 400 g of ice water for dilution.
[0027] The dilute solution was heated to 5°C for hydrolysis reaction. The hydrolysis time was 30 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, and the dichloromethane phase was dried with anhydrous magnesium sulfate and concentrated to obtain 137 g of dinitroamine with a yield of 66.9%. ≥99.5%.
Embodiment 3
[0029] Dissolve 132g of N,N'-diethylurea in 200mL of dichloromethane to prepare a solution, slowly add it to 260g of concentrated nitric acid with a mass concentration of 98% and 218g of 20% oleum to form a mixed acid for nitration reaction, the reaction temperature -5°C to 0°C. After the addition, the reaction mixture was poured into 400 g of ice water for dilution.
[0030] The dilute solution was heated to 25°C for hydrolysis reaction. The hydrolysis time was 80 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, the dichloromethane phase was dried with anhydrous magnesium sulfate, and concentrated to obtain 151 g of dinitroamine, with a yield of 73.8%. ≥99.2%.
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