The preparation method of methylnitrosamine
A technology of metronitramine and concentrated nitric acid, which is applied in the preparation of organic compounds, preparation of urea derivatives, chemical instruments and methods, etc. It can solve problems such as harsh hydrolysis conditions, incomplete nitration of dimethyl urea, and complicated reaction steps , to achieve the effect of increasing the yield
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Embodiment 1
[0017] Dissolve 100g of N,N'-dimethylurea 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 diluted liquid was heated to 20°C for hydrolysis reaction, the hydrolysis time was 60min, after the reaction was terminated, the hydrolyzed liquid phase was separated, the dichloromethane phase was dried with anhydrous magnesium sulfate, and concentrated to obtain 154g of metronitroamine, with a yield of 89.2% and a purity of ≥99.4%.
[0019] Structural Identification of Metronitramine:
[0020] Elemental Analysis:CH 4 N 2 o 2 , calculated: C 15.79, H 5.263, N 36.84;
[0021] Found: C 16.16, H 5.312, N 37.28.
[0022] IR(KBr),υ / cm -1 : 2950, 2898, 1574, 1336, 775, 738.
[0023] 1 H NMR (CD...
Embodiment 2
[0026] Dissolve 100g of N,N'-dimethylurea in 200mL of dichloromethane to prepare a solution, slowly add it to 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 liquid was heated to 5°C for hydrolysis reaction, the hydrolysis time was 30min, after the reaction was terminated, the hydrolyzed liquid phase was separated, the dichloromethane phase was dried with anhydrous magnesium sulfate, and concentrated to obtain 119g of metronitroamine with a yield of 68.9% and a purity of ≥98.7%.
Embodiment 3
[0029] Dissolve 100g of N,N'-dimethylurea in 200mL of dichloromethane to prepare a solution, slowly add 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 diluted liquid was heated to 25°C for hydrolysis reaction, the hydrolysis time was 80min, after the reaction was terminated, the hydrolyzed liquid phase was separated, the dichloromethane phase was dried with anhydrous magnesium sulfate, and concentrated to obtain 150g of metronitroamine with a yield of 86.9% and a purity of ≥99.4%.
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