A kind of preparation method of azasetron hydrochloride
A technology of azasetron hydrochloride and aminoquinuclidine hydrochloride, which is applied in the field of medicine, can solve problems such as difficult removal of by-products, environmental and equipment pollution, unfavorable production methods, etc., to achieve mild reaction conditions, avoid pollution, and yield high rate effect
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Embodiment 1
[0080] In a 500ml three-necked flask, add 150ml of water and 12g (0.3mol) of sodium hydroxide, stir until the solid is completely dissolved, then add 100ml of ethanol, cool down to 20°C, add 6-chloro-4-methyl-3,4-di Hydrogen-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid methyl ester 25.5g (0.1mol), stirring reaction for 3h, the reaction is completed, cooling below 10°C, dilute hydrochloric acid to adjust the pH value to 2 , filtered, and dried to obtain off-white solid of 6-chloro-4-methyl-3,4-dihydro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, 21.9g, yield The rate is 91%.
[0081] 6-chloro-4-methyl-3,4-dihydro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid (12.0g, 0.05mol), triethyl phosphite ( Add 10.0g, 0.062mol), 2,2'-dithiodibenzothiazole (20.0g, 0.062mol) and tetrahydrofuran (100ml) into a dry reaction flask, stir at room temperature for 1h, and control the temperature in an ice-water bath below 20°C. A solution of triethylamine (8.6ml) in tetrahydrofuran (20ml) was added dr...
Embodiment 2
[0087]In a 500ml three-neck flask, add 200ml of water and 12g (0.3mol) of sodium hydroxide, stir until the solid is completely dissolved, then add 100ml of ethanol, cool down to 21°C, add 6-chloro-4-methyl-3,4-di Hydrogen-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid methyl ester 25.5g (0.1mol), stirred for 3h, the reaction was completed, cooled below 10°C, dilute hydrochloric acid to adjust the pH value to 1 ~2, filtered and dried to give off-white solid of 6-chloro-4-methyl-3,4-dihydro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, 20.9g , yield 86.7%.
[0088] 6-chloro-4-methyl-3,4-dihydro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid (12.0g, 0.05mol), triethyl phosphite ( Add 9.7g, 0.06mol), 2,2'-dithiodibenzothiazole (19.4g, 0.06mol) and tetrahydrofuran (100ml) into a dry reaction flask, stir at room temperature for 1h, and control the temperature in an ice-water bath below 20°C. A solution of triethylamine (8.6ml) in tetrahydrofuran (20ml) was added dropwise. After dropping, r...
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