Preparation method of para aminoacet anilide
The technology of aminoacetanilide and nitroacetanilide is applied in the field of preparation of p-aminoacetanilide, can solve the problems of complicated preparation method, low product purity and high production cost, and achieves easy industrial production, high reduction yield and high production cost. low effect
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[0025] A preparation method of p-aminoacetanilide, the preparation steps are as follows:
[0026] ① Add p-nitroaniline and glacial acetic acid into the reaction kettle, mix well to obtain a mixed solution, the molar ratio of p-nitroaniline and glacial acetic acid is 1:4-8;
[0027] ②Heat the mixed solution in step ① to 120-130°C, and conduct heat preservation and distillation under normal pressure reflux for 18-20 hours to obtain the reaction solution;
[0028] ③After step ②, the reaction solution is completely dissolved and cooled, filtered, washed, and dried to obtain p-nitroacetanilide, and the obtained acetic acid filtrate is dehydrated and reused;
[0029] ④Put p-nitroacetanilide, catalyst and organic solvent into the autoclave, replace with nitrogen and hydrogen respectively, stir and heat up to 40-100°C, then fill with hydrogen to 0.5-1.5MPa, keep pressure and keep warm for 0.5-2 hours, to obtain p-aminoacetanilide solution, the mass ratio of p-nitroacetanilide to orga...
Embodiment 1
[0037] Embodiment 1, concrete steps are:
[0038] ①Add 36kg of p-nitroaniline and 78.5kg of glacial acetic acid into the reaction kettle, and stir evenly to obtain a mixed solution;
[0039] ②Heating the mixed solution to 120°C, under normal pressure and reflux for heat preservation and distillation for 20 hours to obtain the reaction solution;
[0040] 3. After the reaction solution is completely reacted, cool down, filter, wash, and dry to obtain 46 kg of p-nitroacetanilide, and reuse the obtained acetic acid filtrate after dehydration;
[0041] ④Add 5kg of palladium carbon, 276kg of methanol and 46kg of p-nitroacetanilide into the autoclave, close the autoclave, then replace it with nitrogen 3 times and hydrogen 3 times, stir and heat up to 60°C, then fill with hydrogen, the pressure of hydrogen is 1MPa , pressurized and heat-preserved for 1 hour to obtain p-aminoacetanilide solution;
[0042] ⑤ Filter the p-aminoacetanilide solution at 50°C, distill methanol, and after c...
Embodiment 2
[0044] Embodiment 2, concrete steps are:
[0045] ①Add 36kg of p-nitroaniline and 63kg of glacial acetic acid into the reaction kettle, and stir evenly to obtain a mixed solution;
[0046] ②Heating the mixed solution to 130°C, under normal pressure and reflux for heat preservation and distillation for 18 hours to obtain the reaction solution;
[0047] 3. After the reaction solution is completely reacted, the temperature is lowered, filtered, washed, and dried to obtain 44 kg of p-nitroacetanilide, and the obtained acetic acid filtrate is dehydrated and reused;
[0048] ④Add 6kg of Raney nickel, 230kg of isopropanol and 44kg of p-nitroacetanilide into the autoclave, close the autoclave, then replace with nitrogen 3 times, hydrogen 3 times, stir and heat up to 40°C, then fill with hydrogen, hydrogen The pressure is 0.5MPa, and the pressure-holding and heat-insulating reaction is carried out for 0.5 hours to obtain p-aminoacetanilide solution;
[0049] ⑤ Filter the p-aminoaceta...
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