Method for preparing N-methyl-N', N'-diphenylcarbamide
A technology of diphenylurea and methyl, applied in the field of N-methyl-N', can solve the problems of waste of resources, cumbersome process, high toxicity of raw materials, etc., and achieve stable and reliable product quality, stable reaction process, and short reaction time. Effect
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Embodiment 1
[0026] Add 169.0g (1mol) of diphenylamine, 800mL of toluene, 40g (1.0mol) of sodium hydroxide and 0.5g (0.0015mol) of magnesium octanoate into a three-necked flask equipped with a reflux condenser, an electric stirrer and a thermometer, stir and heat to 70 ℃, after the diphenylamine is completely dissolved, add dropwise a mixture of 115.5g (1.5mol) carbamoyl fluoride and 150mL toluene at a rate of 5mL / min. h. Heating was stopped, the reaction solution was stirred and cooled to 0°C, and white crystals were precipitated. The reaction solution was filtered, the solid matter was taken, washed three times with 300 mL of pure water, and dried to obtain the crude AK-II. The reaction yield is 96.7%. The crude product was recrystallized from methanol to obtain fine product.
Embodiment 2
[0028] Add 169.0g (1mol) of diphenylamine, 500mL of xylene, 177.0g (3.0mol) of trimethylamine and 2.8g (0.01mol) of magnesium naphthenate into a three-necked flask equipped with a reflux condenser, electric stirring and a thermometer, stir, Heat to 75°C, after the diphenylamine is completely dissolved, add dropwise a mixture of 276.0g (2mol) carbamoyl bromide and 200mL toluene at a rate of 5mL / min, after the addition is complete, raise the temperature to 119°C, and reflux for 2 hours. Stop heating, stir, and cool the reaction solution to -3°C, white crystals are precipitated. The reaction solution was filtered, the solid matter was taken, washed four times with 400 mL of pure water, and dried to obtain the crude AK-II. The reaction yield is 96.3%. The crude product was recrystallized from ethanol to obtain the refined product.
Embodiment 3
[0030] Add 169.0g (1mol) diphenylamine, 900mL carbon tetrachloride, 169.5g (1.5mol) triethylamine and 2.0g (0.005mol) stannous octoate into a three-necked flask with a reflux condenser, an electric stirrer and a thermometer, and stir , Heating to 70°C, after the diphenylamine is completely dissolved, add dropwise a mixture of 149.6g (1.6mol) carbamoyl chloride and 160mL toluene at a rate of 5mL / min, after the addition is complete, heat to 108°C, and reflux for 2.5 h. Stop heating, stir, and cool the reaction solution to -3°C, white crystals are precipitated. The reaction solution was filtered, the solid matter was taken, washed three times with 400 mL of pure water, and dried to obtain the crude AK-II. The reaction yield is 96.1%. The crude product was recrystallized from ethyl acetate to obtain fine product.
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