Method for synthesizing ketazine through hydrogen peroxide oxidation method
A technology of hydrogen peroxide and ketazine is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalyst, preparation of imino compounds, etc., and can solve the problems of high cost and large amount of ammonium salt, etc. Achieve the effect of low cost, high catalytic activity and less catalyst dosage
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Embodiment 1
[0034] Into the reactor equipped with stirring, thermometer, ammonia dropper, and reflux condenser, add 79.7g of acetamide, 30g of sodium acetate, 30ml of water, 0.2g of disodium edetate, and 0.1g of disodium hydrogen phosphate , 66.3ml of acetone, 25ml of 51% hydrogen peroxide aqueous solution, stirring to dissolve and start heating, when the temperature of the system reaches 50°C, slowly add 118ml of 26% ammonia water dropwise, and the dripping is completed within 2 hours. Then control the system temperature at 50-65°C for 4 hours. After the reaction is finished, the content of the material is analyzed after cooling down. The calculated yield of acetonazine is 58.7%, and the selectivity of hydrogen peroxide is 68.5%.
Embodiment 2
[0036] Into the reactor equipped with stirring, thermometer, ammonia inlet pipe and reflux condenser, add 127g of acetamide, 1.9g of acetic acid, 10g of 25% aqueous solution of tetramethylammonium hydroxide, 16ml of water, diethylenediaminetetraacetic acid Sodium 0.2g, disodium hydrogen phosphate 0.5g, methyl ethyl ketone 76ml, stir to dissolve and start heating, at the same time pass ammonia, until saturated (gas escapes from the liquid surface), change to slowly pass ammonia, heat up to 43 ° C slowly drop Add 25 ml of 51.3% hydrogen peroxide aqueous solution. Control the system temperature at 50-65°C for 6 hours. After the reaction was completed, the oil phase and the water phase were analyzed respectively. The yield of butanoneazine was calculated to be 83.4%, and the selectivity of hydrogen peroxide was 89.5%.
Embodiment 3
[0038]Into the reactor equipped with stirring, thermometer, ammonia inlet tube and reflux condenser, add 127g of acetamide solution, 1g of guanidine acetate, 35ml of water, 0.2g of disodium edetate, and 0.5g of disodium hydrogen phosphate , methyl ethyl ketone 75.7ml, stir to dissolve and start heating, pass ammonia at the same time, change to slowly pass ammonia after reaching saturation (gas escapes from the liquid surface), and slowly add 25ml of 49.4% hydrogen peroxide solution dropwise when heating to 43°C . Control the system temperature at 50-65°C for 6 hours. After the reaction was completed, the oil phase and the water phase were analyzed respectively. The yield of butanoneazine is 84.2%, and the selectivity of hydrogen peroxide is 88.4%.
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