Energetic ion salt of n-nitrotrinitroethylcarbamate, preparation method and application
A technology of nitrotrinitroethyl carbamate and ionic salt, which is applied in the field of energetic materials, can solve the problems of low oxygen balance, low oxygen balance and low energy of energetic ionic salts, and achieves the effect of simple method
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Embodiment 1
[0015] Example 1 Preparation of N-nitrotrinitroethyl carbamate ammonium salt (1)
[0016] Its structural formula is as follows:
[0017]
[0018] After dissolving 100.3 mg of N-nitrotrinitroethyl carbamate (0.37 mmol) in 2 mL of dichloromethane, 17.9 mg of ammonium carbonate (0.18 mmol) was added to it with stirring, and the reaction was stirred at room temperature for 5 hours, and white precipitated out The solid, the precipitate was filtered, washed with dichloromethane, and dried to obtain 107.9 mg of product. 1 H NMR([D 6 ]DMSO,300MHz):δ=7.24(s,1H), 7.08(s,1H), 6.91(s,1H), 5.58(s,2H)ppm; 13 C NMR([D 6 ]DMSO,100MHz):δ=156.6,125.4,60.6ppm.IR(KBr):3115.9,2360.2,2341.2,1720.7,1596.8,1424.6,1400.5,1304.9,1230.0,1118.0,1093.7,787.4,667.9cm -1 .Elemental analysis for C 3 H 6 N 6 O 10 (286.01): Calculated: C: 12.59H: 2.11N: 29.37; Measured: C: 12.05H: 2.39N: 29.49.
Embodiment 2
[0019] Example 2 Preparation of N-nitrotrinitroethylcarbamate guanidine salt (2)
[0020]
[0021] After dissolving 134.5 mg of N-nitrotrinitroethyl carbamate (0.50 mmol) in 2 mL of dichloromethane, 44.8 mg of guanidine carbonate (0.25 mmol) was added to it under stirring, and the reaction was stirred at room temperature for 3 hours. A white solid precipitated, the precipitate was filtered, washed with dichloromethane, and dried to obtain the product in a quantitative yield. 1 H NMR([D 6 ]DMSO, 300MHz): δ = 6.90 (s, 6H), 5.58 (s, 2H) ppm; 13 C NMR([D 6 ]DMSO,100MHz):δ=158.0,157.4,125.6,60.5ppm.IR(KBr):3445.9,3273.4,3206.8,3012.8,2951.4,1716.7,1662.7,1593.2,1432.2,1382.5,1304.1,1222.5,1113.4,1036.6, 967.0, 885.5, 856.1, 811.9, 784.0, 539.6cm -1 .Elementalanalysis for C 4 H 8 N 8 O 10 (328.04):Calculated:C:14.64H:2.46N:34.15; Measured:C:14.78H:2.65N:34.30.
Embodiment 3
[0022] Example 3 Preparation of N-nitrotrinitroethyl carbamate-aminoguanidine salt (3)
[0023] Its structural formula is as follows:
[0024]
[0025] After dissolving 301.2 mg of N-nitrotrinitroethyl carbamate (1.10 mmol) in 2 mL of methanol, 155.5 mg of guanidine bicarbonate (1.10 mmol) was added to it under stirring. The reaction was stirred at room temperature for 1 hour, and concentrated to remove Solvent, 385.2 mg of product was obtained in a quantitative yield. 1 H NMR([D 6 ]DMSO,300MHz):δ=8.56(s,2H),7.26(s,2H),6.73(s,2H),5.59(s,2H),4.42(s,2H)ppm; 13 C NMR([D 6 ]DMSO,100MHz):δ=158.80,156.76,125.60,60.57ppm.IR(KBr):3507.96,3422.99,3392.06,3332.36,3241.02,2990.41,2952.48,2894.16,2359.92,2340.02,2191.85,1686.94,1667.12,1581.04, 1530.27,1418.50,1384.86,1301.66,1231.97,1116.29,1089.29,959.40,855.38,822.03,786.10,739.89,667.79,547.35,437.48cm -1 .Elemental analysis for C 4 H 9 N 9 O 10 (343.05):Calculated:C:14.00H:2.64N:36.73; Measured:C:14.11H:2.70N:36.68.
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