Purification method of omeprazole
A technology of omeprazole and omeprazole sodium, applied in the direction of organic chemistry, etc., can solve the problems of poor purity of omeprazole, affecting clinical application, and decreased stability of omeprazole preparations, etc.
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Embodiment 1
[0014] 20g omeprazole, 10g3, the 5-dichloronitrobenzene crude product is dissolved in 100ml acetonitrile / 20% methylamine trichloromethane mixed solvent, the mixing ratio of acetonitrile, 20% methylamine trichloromethane solution is 1: 1, temperature Raised to 50 degrees Celsius, maintained for 5 hours, during which the stirring continued;
[0015] Adjust the pH to 9.0 with sodium bicarbonate, lower the temperature to 0°C, and keep it for 1 hour to precipitate a solid, wash it with deionized water after centrifugation, and dry it in vacuum at 30°C for 5 hours. Obtained 18g of fine omeprazole with a purity of 99.5%.
Embodiment 2
[0017] 20g omeprazole, 10g3, the 5-dichloronitrobenzene crude product is dissolved in 100ml acetonitrile / 20% methylamine trichloromethane mixed solvent, the mixing ratio of acetonitrile, 20% methylamine trichloromethane solution is 1: 1, temperature Raised to 60 degrees Celsius, maintained for 6 hours, during which the stirring continued;
[0018] Sodium bicarbonate adjusted the pH to 11.0, lowered the temperature to 4 degrees Celsius, and kept it for 2 hours to precipitate a solid, washed with deionized water after centrifugation, and dried in vacuum at 40 degrees Celsius for 7 hours. Obtained 17.8 g of refined omeprazole with a purity of 99.3%.
Embodiment 3
[0020] 20g of omeprazole and 16g of crude 3,5-dichloronitrobenzene were dissolved in 100ml of solvent A, the temperature was raised to 60 degrees Celsius, and maintained for 6 hours, during which the stirring was continued;
[0021] Sodium bicarbonate adjusted the pH to 11.0, lowered the temperature to 4 degrees Celsius, and kept it for 2 hours to precipitate a solid, washed with deionized water after centrifugation, and dried in vacuum at 40 degrees Celsius for 7 hours. Get omeprazole boutique.
[0022] Solvent A is selected from acetonitrile / 20% methylamine chloroform mixed solvent (1:1), chloroform, acetonitrile, acetonitrile / 20% methylamine chloroform mixed solvent (2:1), acetonitrile / 20% methylamine Chloroform mixed solvent (2:1), acetonitrile / 20% methylamine chloroform mixed solvent (3:1), acetonitrile / 20% methylamine chloroform mixed solvent (1:2), acetonitrile / 20% methylamine Amine trichloromethane mixed solvent (1:3), the experimental results are shown in the table b...
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