Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene
A technology of dinitrophenoxy and dinitro, which is applied in 1 field to achieve the effects of simple operation, convenient recycling, and less waste
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Embodiment 1
[0027] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 64.8 grams (0.32 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N- Put dimethylformamide and 180 ml of toluene into the reaction kettle, stir, heat and reflux for water separation for 18 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate a solid product, wash and dry , obtain 58.2 grams of 1,3,5-three (2,4-dinitrophenoxy) benzene crystal products, the purity is 99.0%, according to the actual acquisition of 1,3,5-three (2,4-dinitrophenoxy) The yield of 1,3,5-tri(2,4-dinitrophenoxy)benzene was calculated to be 93.2%.
Embodiment 2
[0029] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 0.32 moles of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N,N-dimethylethane Amide and 15 milliliters of dimethylbenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 6 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed and dried to obtain 1 , 3,5-tris(2,4-dinitrophenoxy)benzene crystal product, according to the actual amount and theoretical amount of 1,3,5-tris(2,4-dinitrophenoxy)benzene obtained (62.4 g), the calculated yield of 1,3,5-tris(2,4-dinitrophenoxy)benzene was 87.3%.
Embodiment 3
[0031] 12.6 grams (0.10 moles) of 1,3,5-pyrroglucinol, 0.30 moles of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 80 milliliters of N-methyl-2-pyrrolidone and 30 milliliters of dichlorobenzene were put into a reaction kettle, stirred, heated to reflux and separated from water for 16 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed, dried, and obtained 1,3,5-tris(2,4-dinitrophenoxy)benzene crystal product, according to the actual amount of 1,3,5-tris(2,4-dinitrophenoxy)benzene obtained and Theoretical yield (62.4 g), the calculated yield of 1,3,5-tris(2,4-dinitrophenoxy)benzene was 88.1%.
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