Method for preparing 1,5-di(2,4-dinitrophenoxy)naphthalene
A technology of dinitrophenoxy and dinitro, which is applied in 1 field to achieve the effects of high product yield and purity, fewer types of use, and convenient recovery
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Embodiment 1
[0026] 16.0 grams (0.10 moles) of 1,5-naphthalenediol, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N-dimethyl Put formamide and 180ml 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 the solid product, wash with hot water for 2 to 3 times, dry to obtain 47.3 grams of 1,5-bis(2,4-dinitrophenoxy)naphthalene crystal product with a purity of 99.1%, and obtain 1,5-bis(2,4-dinitro According to the amount of phenoxy)naphthalene and the theoretical amount (49.2 grams), the calculated yield of 1,5-bis(2,4-dinitrophenoxy)naphthalene is 96.1%.
Embodiment 2
[0028] 16.0 grams (0.10 moles) of 1,5-naphthalenediol, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 50 milliliters of N-methyl-2- Pyrrolidone, 150 milliliters of N,N-dimethylacetamide 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, Add water to precipitate a solid product, wash with hot water for 2 to 3 times, and dry to obtain 38.5 grams of 1,5-bis(2,4-dinitrophenoxy)naphthalene crystal product with a purity of 99.0%. According to the actual obtained 1, The amount and theoretical amount (49.2 grams) of 5-bis(2,4-dinitrophenoxy)naphthalene, calculate the yield of 1,5-bis(2,4-dinitrophenoxy)naphthalene as 78.2%.
Embodiment 3
[0030] 16.0 grams (0.10 moles) of 1,5-naphthalenediol, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 80 milliliters of N-methyl-2- Pyrrolidone and 30 ml of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 16 hours, then concentrated the reaction liquid, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed with hot water for 2 ~ 3 times, dried to obtain 35.5 grams of 1,5-bis(2,4-dinitrophenoxy)naphthalene crystal product with a purity of 98.9%. According to the actual obtained 1,5-bis(2,4-bis According to the amount of nitrophenoxy)naphthalene and the theoretical yield (49.2 grams), the calculated yield of 1,5-bis(2,4-dinitrophenoxy)naphthalene was 72.1%.
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