Preparation method of 4-ethyl aminobenzoate powder
A technology of ethyl aminobenzoate and aminobenzoic acid, which is applied in the field of preparation of 4-aminobenzoic acid ethyl ester powder, can solve the problems of low production capacity, high energy consumption, easy generation of dust, etc., and achieves high production capacity and energy consumption. Low, pollution-reducing effect
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Embodiment 1)
[0020] The preparation method of the ethyl 4-aminobenzoate powder of the present embodiment is as follows:
[0021] ①Add 40g of 4-nitrobenzoic acid, 200mL of water, 0.5g of 4-dimethylaminopyridine and 0.6g of 3wt% palladium carbon catalyst into the autoclave, first replace it with nitrogen three times, then feed hydrogen and adjust the pressure to 0.8±0.1MPa, and at the same time control the temperature at 100±2°C, heat preservation and pressure to complete the reaction.
[0022] After the reaction, the catalyst was recovered by filtration, the filtrate was cooled, crystallized, filtered, and dried under vacuum at 80-85°C to obtain 32.0 g of 4-aminobenzoic acid with a yield of 97.5%, a melting point of 187.0-187.5°C, and a content of 99.9 % (permanent stop titration).
[0023] ②Add 200mL of ethanol to the reaction bottle and keep the temperature at 25±5℃, then add 27g of 98wt% concentrated sulfuric acid dropwise, and then add 30g of 4-aminobenzoic acid, heat to reflux and com...
Embodiment 2)
[0041] The preparation method of the ethyl 4-aminobenzoate powder of the present embodiment is as follows:
[0042] ①Add 60g of 4-nitrobenzoic acid, 300mL of water, 1.0g of 4-dimethylaminopyridine and 1.1g of 3wt% palladium carbon catalyst into the autoclave, first replace it with nitrogen three times, then feed hydrogen and adjust the pressure to 0.8±0.1MPa, and at the same time control the temperature at 100±2°C, heat preservation and pressure to complete the reaction.
[0043] After the reaction, the catalyst was recovered by filtration, the filtrate was cooled, crystallized, filtered, and dried under vacuum at 80-85°C to obtain 47.7g of 4-aminobenzoic acid with a yield of 96.9%, a melting point of 187.1-187.6°C, and a content of 100.2 % (permanent stop titration).
[0044] ②Add 260mL of ethanol to the reaction bottle and keep the temperature at 25±5℃, then add 38g of 98wt% concentrated sulfuric acid dropwise, and then add 45g of 4-aminobenzoic acid, heat to reflux and com...
Embodiment 3)
[0049] The preparation method of the ethyl 4-aminobenzoate powder of the present embodiment is as follows:
[0050]①Add 60g of 4-nitrobenzoic acid, 300mL of water, 1.0g of 4-dimethylaminopyridine and 1.1g of 3wt% palladium carbon catalyst into the autoclave, first replace it with nitrogen three times, then feed hydrogen and adjust the pressure to 0.8±0.1MPa, and at the same time control the temperature at 100±2°C, heat preservation and pressure to complete the reaction.
[0051] After the reaction, the catalyst was recovered by filtration, the filtrate was cooled, crystallized, filtered, and dried under vacuum at 80-85°C to obtain 47.7g of 4-aminobenzoic acid, the yield was 96.9%, the melting point was 186.9-187.5°C, and the content was 99.8 % (permanent stop titration).
[0052] ② Add 260mL of ethanol to the reaction bottle and keep the temperature at 25±5°C, then add 38g of 98wt% concentrated sulfuric acid dropwise, and then add 45g of 4-aminobenzoic acid, heat to reflux an...
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