Method for preparing N,N-diethyl M-Methyl Benzoyl amide
A technology of methyl benzamide and methyl benzoyl chloride, applied in the N field, can solve the problems of many impurities, long production time, and many production equipment, and achieve the effects of wide source of raw materials, improved production efficiency and low price
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[0019] Example 1
[0020] A preparation method of N,N-diethyl m-methylbenzamide, the steps are as follows:
[0021] (1) Amidation reaction steps
[0022] Put 80 kg of ethylenediamine, 104 kg of water and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring and thermometer. Under stirring, 160 kg of m-toluyl chloride and acid absorption are added at the same time. 46 kg of refined sodium hydroxide, keep the reaction at room temperature, after the materials are added, stir and react for 1.5 hours, and the reaction is complete;
[0023] Mid-term: The weight ratio of acid absorption refined preparation: m-toluyl chloride is 0.28-0.35:1;
[0024] The weight ratio of m-methylbenzoyl chloride: diethylamine: water: benzene is 1:0.5:0.65:1.25.
[0025] (2) Washing steps
[0026] Add 40 kilograms of water for washing to the oil layer mixture obtained after the amidation reaction, stir evenly, stand still for layering, and remove the water layer;
[0027] The ...
Example Embodiment
[0030] Example 2
[0031] A preparation method of N,N-diethyl m-methylbenzamide, the steps are as follows:
[0032] (1) Amidation reaction steps
[0033] Put 80 kg of ethylenediamine, 104 kg of water and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring and thermometer. Under stirring, 160 kg of m-toluyl chloride and acid absorption are added at the same time. 48 kg of refined sodium hydroxide, keep the reaction at room temperature, after the materials are added, stir and react for 1.5 hours, the reaction is complete;
[0034] (2) Washing steps
[0035] Add 40 kilograms of water for washing to the oil layer mixture obtained after the amidation reaction, stir evenly, stand still for layering, and remove the water layer;
[0036] (3) Distillation and solvent removal step
[0037] The water-washed mixed liquid is distilled to remove the solvent benzene. The temperature of the distillation is below 85°C and the vacuum degree is 10-15mmHg. The remain...
Example Embodiment
[0038] Example 3
[0039] A preparation method of N,N-diethyl m-methylbenzamide, the steps are as follows:
[0040] (1) Amidation reaction step
[0041] Put 80 kg of ethylenediamine, 104 kg of water and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring and thermometer. Under stirring, 160 kg of m-toluyl chloride and acid absorption are added at the same time. 50 kg of refined sodium hydroxide, keep the reaction at room temperature, after the materials are added, stir and react for 1.5 hours, and the reaction is complete;
[0042] (2) Washing steps
[0043] Add 40 kilograms of water for washing to the oil layer mixture obtained after the amidation reaction, stir evenly, stand still for layering, and remove the water layer;
[0044] (3) Distillation and solvent removal step
[0045] The water-washed mixed liquid is distilled to remove the solvent benzene. The temperature of the distillation is below 85°C and the vacuum degree is 10-15mmHg. The rem...
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