Preparation of 4-aminobenzoic acid (4-aminophenyl)-ester
A technology of aminobenzoic acid and aminophenyl, which is applied in the field of preparation of 4-aminobenzoic acid ester, can solve difficult problems and achieve the effects of low production cost, strong market competitiveness, and low environmental pollution
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[0020] Example 1:
[0021] In a 500 ml three-necked flask, add 56 g of p-nitrophenol, 43 g of p-nitrobenzoyl chloride, 350 ml of dimethylformamide, and 3 g of KI. Start stirring and raise the temperature to 140°C to perform the heat preservation and reflux reaction. The generated HCl gas is water Absorb into a hydrochloric acid solution, react for 8 hours until the reaction is completely stopped, cool down until the product precipitates out crystals, and filter with suction. The filter cake is a light yellow sandy particle dinitro intermediate, and the component of the dinitro intermediate 4-nitro 4-nitrophenyl benzoate, which can be directly used in the next hydrogenation reaction. The purity of 4-nitro benzoate (4-nitrophenyl) is 98.5%. The entire condensation reaction The yield of HCl is 97%, and the melting range of the dinitro intermediate is 160-163°C, which prevents HCl from siphoning during the water absorption process.
[0022] Add 40g of dinitro intermediate, 200ml of di...
Example Embodiment
[0023] Example 2:
[0024] In a 500 ml three-necked flask, add 56 g of p-nitrophenol, 48 g of p-nitrobenzoyl chloride, 250 ml of xylene, and 3 g of dimethylaminopyridine DMAP catalyst. Start stirring and raise the temperature to 135°C, and carry out the reflux reaction with heat preservation. The produced HCl The gas is absorbed into a hydrochloric acid solution with water. After 3 hours of reaction, the reaction is completely stopped, and the temperature is cooled until the product precipitates crystals for suction filtration. The filter cake is a light yellow sand-like particle dinitro intermediate, 4-nitrobenzoic acid (4 The purity of the -nitrophenyl) ester is 98%, and the yield of the entire condensation reaction is 93%, which prevents siphoning during the absorption of HCl water.
[0025] Add 40g of dinitro intermediate, 150ml of ethanol, and 5g of Pd / C catalyst with 3% palladium content into the autoclave, stir and raise the temperature to 80°C and the pressure to 2.0MPa fo...
Example Embodiment
[0026] Example 3:
[0027] In a 500 ml three-necked flask, add 56 g of p-nitrophenol, 38 g of p-nitrobenzoyl chloride, 150 ml of toluene, and 2 g of catalyst KCl. Start stirring and raise the temperature to 115°C to perform the reflux reaction. The generated HCl gas is absorbed into hydrochloric acid with water. Solution, after the reaction is completed for 3 hours, stop the reaction, cool down until the product precipitates crystals, and filter with suction. The filter cake is a light yellow sand-like particle dinitro intermediate. The yield of the entire condensation reaction is 93%, the dinitro intermediate The melting range of the body is 160~163℃.
[0028] Add 40g of dinitro intermediate, 250ml of methanol, and 0.5g of Raney-Ni catalyst into the autoclave, stir and raise the pressure to 80°C and 0.8MPa for catalytic hydrogenation reaction, filter the Raney-Ni catalyst, and distill the filtrate to obtain The yellow loose product 4-aminobenzoic acid (4-aminophenyl) ester, with ...
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