A melting and casting explosive 3,4,5-trifluoro-2,6-dinitroaniline and its preparation method and application
A technology of dinitroaniline and casting explosives, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of ammunition sensitivity, fragility and transportation impact, workers' health and environmental hazards, explosives Oil leakage and other problems, to achieve the effect of superior performance, safe raw materials, and easy recrystallization
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Embodiment 1
[0024] Preparation of starting material 1:
[0025] With an ice-water bath and magnetic stirring, after dissolving 14.7 grams (0.1mol) of trifluoroaniline with 150 milliliters of acetonitrile, add 11.11 grams (0.11mol) of triethylamine, and then slowly add an acylating agent (such as acetyl chloride, Acetic anhydride, methyl chloroformate or ethyl chloroformate) (0.11mol), after the dropwise addition, the stirring was continued at room temperature until the reaction was complete (TLC detection).
[0026] After the reaction was complete, the reaction system was slowly poured into ice water, a large amount of precipitates were precipitated, and the raw material 1 was obtained by filtration, and the yield was quantitative.
[0027] When the acylating reagent is acetyl chloride or acetic anhydride, the raw material 1 shown in formula II is obtained, where R=CH 3 CO; when the acylating reagent is methyl chloroformate, the raw material 1 shown in formula II is obtained, where R=CH ...
Embodiment 2
[0029] A kind of preparation of melting and casting explosive 3,4,5-trifluoro-2,6-dinitroaniline (ZXC-17), comprising the following steps:
[0030] Accurately weigh 11.11 grams of potassium nitrate (110mmol, 2.2eq), and slowly add it to 50 ml of concentrated sulfuric acid (concentration of sulfuric acid is 95-98%) under ice-water bath and magnetic stirring conditions, and continue to stir until the potassium nitrate is completely Dissolve, and then slowly add raw material 1 (50mmol, 1.0eq). After the addition, the system was slowly raised to room temperature and continued to stir until the reaction was complete (TLC detection).
[0031] After the reaction was complete, the reaction mixture was slowly poured into ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain an orange-yellow solid with a yield of 87.92%; the H NMR spectrum of the product was 1 H NMR (600MHz, DMSO-d 6 ,TMS,ppm), δ=8.63(s,2H); 13 C NMR (125MHz, DMS...
Embodiment 3
[0033] A kind of preparation of melting and casting explosive 3,4,5-trifluoro-2,6-dinitroaniline (ZXC-17), comprising the following steps:
[0034]Accurately weigh 8.8 grams of ammonium nitrate (110mmol, 2.2eq), and slowly add it to 50 milliliters of concentrated sulfuric acid (concentration of sulfuric acid is 95-98%) under conditions of ice-water bath and magnetic stirring, and continue to stir until the potassium nitrate is completely Dissolve, and then slowly add raw material 1 (50mmol, 1.0eq). After the addition, the system was slowly raised to room temperature and continued to stir until the reaction was complete (TLC detection).
[0035] After the reaction was complete, the reaction mixture was slowly poured into ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain an orange-yellow solid with a yield of 86.54%.
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Abstract
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