A heat-resistant compound 2-fluro-1,3,5-triamino-4,6-dinitrobenzene and a preparing method thereof
A technology for dinitrobenzene and dinitroaniline, which is applied in the field of compound preparation, can solve the problems of insufficient stability of explosives, easy evaporation and the like, and achieves the effects of superior performance, easy recrystallization and simple equipment
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Embodiment 1
[0029] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:
[0030] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:
[0031] Under magnetic stirring, add 125mmol potassium nitrate and 10.95 grams of N-ethylcarbonate-3,4,5-trifluoroaniline (50mmol) successively in 100 milliliters of concentrated sulfuric acid (98% by mass) in an ice-water bath, and react After completion, the reaction system was slowly poured into ice water, continued to stir for 1 hour until the system returned to room temperature, filtered, washed, and dried to obtain 11.02 g of a light yellow solid with a yield of 93%. The light yellow solid was 3 ,4,5-Trifluoro-2,6-dinitroaniline.
[0032] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:
[0033] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 50 ml of concentrated ammonia water with a mass perc...
Embodiment 2
[0035] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:
[0036] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:
[0037]Under magnetic stirring, add 10.95 g of N-ethylcarbonate-3,4,5-trifluoroaniline (50 mmol) in 100 ml of concentrated sulfuric acid (98% by mass) in an ice-water bath, then slowly add 15 Milliliter fuming nitric acid (mass percentage is 95%), after the reaction is complete, the reaction system is slowly poured into ice water, continue to stir for 1 hour until the system returns to room temperature, filter, wash, and dry to obtain 10.95 grams of light yellow solid. The yield was 92.4%, and the light yellow solid was 3,4,5-trifluoro-2,6-dinitroaniline.
[0038] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:
[0039] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 50 ml of concentrated ammonia wa...
Embodiment 3
[0041] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:
[0042] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:
[0043] Under magnetic stirring, add 125mmol sodium nitrate and 10.95 grams of N-ethylcarbonate-3,4,5-trifluoroaniline (50mmol) successively in 100 milliliters of concentrated sulfuric acid (98% by mass) in an ice-water bath, and react After completion, the reaction system was slowly poured into ice water, continued to stir for 1 hour until the system returned to room temperature, filtered, washed, and dried to obtain 11.02 g of a light yellow solid with a yield of 93%. The light yellow solid was 3 ,4,5-Trifluoro-2,6-dinitroaniline.
[0044] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:
[0045] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 10 ml of 40% by mass concentrated ammonia water under m...
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