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3-Aminoacetophenone Powder

3 year ago
18 0
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M-aminoacetophenone is an important pharmaceutical and organic intermediate, and its downstream products have important applications. For example, m-hydroxyacetophenone is an intermediate in the synthesis of epinephrine drugs, m-chlorophenone can be used in the synthesis of new special drugs for bronchiectasis, purpura and other drugs, and 3-acetamide acetophenone is an intermediate in the synthesis of sedative and hypnotic drug indineplon. Preparation 2.0g m-nitroacetophenone, 0.2gPT /Bi2O3(Pt content of 0.2wt %) and 10mL absolute methanol were added to 50mL intermittent reaction kettle. Nitrogen and hydrogen were successively used to replace the gas in the reactor for 3-5 times. Hydrogen was filled to the pressure of 1.0mpa, and the temperature was raised to 70℃ under constant agitation. The stirring speed is 600-800 RPM. If the total pressure drops below 0.5MPa, hydrogen is added to the initial pressure. After 4h, the total pressure did not change, and the stirring was stopped and cooled to room temperature. The reaction mixture was centrifuged with a yellow catalyst at the bottom and a green supernatant (if the conversion of m-nitroacetophenone was incomplete, the supernatant was yellow and green, with nitroso-partial hydrogenation products nitroso compounds as by-products). A small amount of the supernatant was analyzed by gas chromatography, and the conversion of m-nitroacetophenone was more than 99.9%, and the selectivity of m-aminophenone was more than 99.9%.
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