A kind of production technology of p-aminobenzamide
A technology of aminobenzamide and production process, which is applied in the field of production technology of p-aminobenzamide, can solve the problems of unfavorable green industrial production of aminobenzamide, high price of acyl chloride reagents, equipment corrosion, etc. Industrialized production, low cost and high total yield
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Embodiment 1
[0035] (1) Preparation of ethyl p-nitrobenzoate
[0036] In a 1000 ml four-neck flask connected with stirring, thermometer, water separator, and reflux condenser, 83.5 grams (0.5 moles) of p-nitrobenzoic acid, 250 grams of ethanol, 1.5 grams of p-toluenesulfonic acid, and 120 grams of toluene , 74.4 ° C (toluene-ethanol-water azeotropic) reflux with water for 7 hours, then cooled to 50-60 ° C, low vacuum and reduced pressure recovery ethanol and toluene (for the next batch of reactions), then high vacuum vacuum distillation ( 5-10mmHg) distilled 94.2 grams of ethyl p-nitrobenzoate, yield 96.5%, GC purity 99.9%.
[0037] (2) Preparation of p-aminobenzamide
[0038] In 500 milliliters of stainless steel autoclaves, add 39.0 grams (0.2 moles) ethyl p-nitrobenzoate prepared by step (1), 200 grams of 10% ammonia methanol solution, 0.3 grams of 5% palladium carbon catalyst, after nitrogen replacement three times, Pass in hydrogen, keep the hydrogen pressure at 0.2-0.3 MPa, and rea...
Embodiment 2
[0041] (1) Preparation of ethyl p-nitrobenzoate
[0042] In the 1000 milliliter four-neck flask that is connected with stirring, thermometer, water separator, reflux condenser, 83.5 grams (0.5 moles) p-nitrobenzoic acid, 230 grams of ethanol, 1.5 grams of solid super acid, 120 grams of normal hexane, 56 ℃ (n-hexane-ethanol-water azeotrope) was refluxed with water for 9 hours, then cooled to 40-50°C, low-vacuum and decompressed to recover n-hexane and ethanol (for the next batch of reactions), and then high-vacuum and reduced-pressure distillation ( 5-10mmHg) distilled 95.7 grams of ethyl p-nitrobenzoate, yield 98.2%, GC purity 99.8%.
[0043] (2) Preparation of p-aminobenzamide
[0044]Get 39.0 grams (0.2 moles) of ethyl p-nitrobenzoate prepared in step (1) and join in 500 milliliters of stainless steel autoclave, and add 200 grams of 10% ammonia ethanol solution, 3.5 grams of 50% Raney nickel catalyst, nitrogen displacement After three times, hydrogen gas was introduced to ...
Embodiment 3
[0046] (1) Preparation of ethyl p-nitrobenzoate
[0047] In a 1000 ml four-necked flask connected with stirring, thermometer, water separator, and reflux condenser, 75.0 grams (0.45 moles) of p-nitrobenzoic acid, 250 grams of ethanol, 1.5 grams of p-toluenesulfonic acid, and 150 grams of petroleum Ether, reflux at 65.5°C (petroleum ether-ethanol-water azeotrope) with water to react for 8 hours, then cool to 50-60°C, recover petroleum ether and ethanol (for the next batch reaction) under low vacuum and decompression, and then reduce Pressure distillation (5-10mmHg) distilled 86.5 grams of ethyl p-nitrobenzoate, yield 98.5%, GC purity 99.9%.
[0048] (2) Preparation of p-aminobenzamide
[0049] In 500 milliliters of stainless steel autoclaves, add 39.0 grams (0.2 moles) ethyl p-nitrobenzoate prepared by step (1), 200 grams of 10% ammonia methanol solution, 0.3 grams of 5% palladium carbon catalyst, after nitrogen replacement three times, Pass in hydrogen, keep the hydrogen pre...
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