4,4-dinitrodiphenyl ethers synthesis method
A technology of dinitrodiphenyl ether and synthesis method, which is applied in 4 fields, can solve the problems of production equipment limitation, difficult industrial production, unfavorable production, etc., and achieve the effect of easy maintenance and use
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Embodiment 1
[0032] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 12g sodium bicarbonate, 100gDMF, 2g ethylene glycol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat Raise the temperature, the reaction temperature is 140°C, and maintain the reaction temperature for 3 hours, stop heating, wait to cool to room temperature, and filter with suction to obtain 4,4'-dinitrodiphenyl ether crystals, and the obtained product is washed with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 25.7g of dry crystalline product with a melting range of 142-143°C. Yield: 98.8%.
Embodiment 2
[0034] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 10g potassium bicarbonate, 100gDMA, 3g butanol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat up , the reaction temperature is 145°C, and keep the reaction temperature for 3.5h, stop heating, wait to cool to room temperature, and filter with suction to obtain 4,4'-dinitrodiphenyl ether crystals, the obtained product is washed with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 25.5g of dry crystalline product with a melting range of 142-143°C. Yield: 98.1%.
Embodiment 3
[0036] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 11g sodium carbonate, 100gDMSO, 2.5g butylene glycol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat Raise the temperature, the reaction temperature is 135°C, and maintain the reaction temperature for 3 hours, stop heating, wait to cool to room temperature, and filter with suction to obtain crystals of 4,4'-dinitrodiphenyl ether, wash the obtained product with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 24.5g of dry crystalline product with a melting range of 142-143°C. Yield: 94.2%.
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