New method of catalyzed synthesis of aspirin
A technology of aspirin and catalyst, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of lowering reaction temperature, high product purity and mild properties
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Embodiment 1
[0032] The method that a kind of novel catalyst synthesis aspirin provided by the present embodiment comprises the following steps:
[0033] Add 6.9g (50mmol) of salicylic acid, 0.552g of tyrosine, and 5.1g (50mmol) of acetic anhydride into a 150mL dry three-necked flask. After mixing, fix it in a water bath of an ultrasonic cleaner at 50°C , the ultrasonic power is 500W, the reaction time is 15min, then remove the three-neck flask from the water bath, wash the inner wall of the flask with ice water, after the crystallization is formed, add a certain amount of water, and place it in an ice-water bath to cool, so that the crystallization is complete, Suction filtration, the filter cake was washed with a small amount of distilled water, and dried to obtain the crude aspirin product in the form of white needles. Add the crude product into a saturated sodium bicarbonate solution, stir until there are no bubbles, filter out the insoluble matter, slowly pour the filtrate into a beak...
Embodiment 2
[0048] The method that a kind of novel catalyst synthesis aspirin provided by the present embodiment comprises the following steps:
[0049] Add 6.9g (50mmol) of salicylic acid, 0.552g of tyrosine, and 10.2g (100mmol) of acetic anhydride into a 150mL dry three-necked flask. After mixing, fix it in a water bath of an ultrasonic cleaner at 50°C , the ultrasonic power is 500W, the reaction time is 5min, then remove the three-neck flask from the water bath, wash the inner wall of the flask with ice water, after the crystallization is formed, add a certain amount of water, and place it in an ice-water bath to cool, so that the crystallization is complete, Suction filtration, the filter cake was washed with a small amount of distilled water, and dried to obtain the crude aspirin product in the form of white needles. Add the crude product into a saturated sodium bicarbonate solution, stir until there are no bubbles, filter out the insoluble matter, slowly pour the filtrate into a bea...
Embodiment 3
[0064] The method that a kind of novel catalyst synthesis aspirin provided by the present embodiment comprises the following steps:
[0065] Add 6.9g (50mmol) of salicylic acid, 0.552g of tyrosine, and 10.2g (100mmol) of acetic anhydride into a 150mL dry three-necked flask. After mixing, fix it in a water bath of an ultrasonic cleaner at 30°C , the ultrasonic power is 500W, the reaction time is 15min, then remove the three-neck flask from the water bath, wash the inner wall of the flask with ice water, after the crystallization is formed, add a certain amount of water, and place it in an ice-water bath to cool, so that the crystallization is complete, Suction filtration, the filter cake was washed with a small amount of distilled water, and dried to obtain the crude aspirin product in the form of white needles. Add the crude product into a saturated sodium bicarbonate solution, stir until there are no bubbles, filter out the insoluble matter, slowly pour the filtrate into a be...
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