Preparation method of rivaroxaban
A technology of rivaroxaban and organic solvents, applied in the field of medicine, can solve problems such as inability to carry out industrial production, incomplete substrate reaction, toxicity yield, etc., and achieve the effect of low cost, simple operation and high yield
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[0031] Example 1:
[0032] a) Preparation of 2-((2R)-2-hydroxy-3-{[4-(3-oxo-4-morpholinyl)phenyl]amino}propyl)-1H-isoindole-1,3 (2H)-Diketone (IV)
[0033] Add absolute ethanol (1.48kg) and process water (467g) to a 3L reaction flask, turn on the stirrer to stir, and then add 4-(4-aminophenyl)-3-morpholinone(II)(62.3) g) and 2-[(2S)-2-oxiranylmethyl]-1H-isoindole-1,3(2H)-2one (III) (65.9g), start heating to 70℃, After reacting for 4 hours, stop heating, cool to 35°C, filter with suction, rinse the solid with 90% ethanol (150g), pump the mother liquor back into the reaction flask, distill 1kg of solvent, and add 2-[(2S)- 2-Ethylene oxide methyl]-1H-isoindole-1,3(2H)-2one(III)(32.9g), heat to 70℃, react for 4 hours, stop heating, and cool to 30℃ , Suction filtration, the solid is rinsed with 90% ethanol (100g), the filtrate is treated as a waste liquid, the solids obtained by the two suction filtrations are combined and dried. 121.8 g of product was obtained, purity: 96%, melting...
Example Embodiment
[0041] Example 2:
[0042] a) Preparation of 2-((2R)-2-hydroxy-3-{[4-(3-oxo-4-morpholinyl)phenyl]amino}propyl)-1H-isoindole-1,3 (2H)-Diketone (IV)
[0043] Add absolute ethanol (1.48kg) and process water (467g) to a 3L reaction flask, turn on the stirrer to stir, and then add 4-(4-aminophenyl)-3-morpholinone(II)(62.3) g) and 2-[(2S)-2-oxiranylmethyl]-1H-isoindole-1,3(2H)-2one (III) (65.9g), start heating to 70℃, React for 4 hours, stop heating, cool to 25°C, filter with suction, rinse the solid with 90% ethanol (150g), pump the mother liquor back into the reaction flask, distill 1kg solvent, and add 2-[(2S)- 2-Ethoxyethylene methyl]-1H-isoindole-1,3(2H)-2one(III)(32.9g), heat to 70℃, react for 4 hours, stop heating, and cool to 35℃ , Suction filtration, the solid is rinsed with 90% ethanol (100g), the filtrate is treated as a waste liquid, the solids obtained by the two suction filtrations are combined and dried. 117.8 g of product was obtained, purity: 90%, melting point: 217°...
Example Embodiment
[0051] Example 3:
[0052] a) Preparation of 2-((2R)-2-hydroxy-3-{[4-(3-oxo-4-morpholinyl)phenyl]amino}propyl)-1H-isoindole-1,3 (2H)-Diketone (IV)
[0053] Add absolute ethanol (1.48kg) and process water (467g) to a 3L reaction flask, start stirring, and then add 4-(4-aminophenyl)-3-morpholinone (II) (62.3g) and 2-[(2S)-2-Ethoxyethylenemethyl]-1H-isoindole-1,3(2H)-2one(III)(65.9g), start heating to 70℃, and react for 4 hours , Stop heating, cool to 35℃, filter with suction, rinse the solid with 90% ethanol (150g), pump the mother liquor back into the reaction flask, distill 1kg of solvent, add 2-[(2S)-2-ring to it Oxyethylene methyl]-1H-isoindole-1,3(2H)-2one(III)(39.54g), heat to 70℃, react for 4 hours, stop heating, cool to 30℃, filter with suction , The solid was rinsed with 90% ethanol (100g), the filtrate was treated as a waste liquid, and the solid obtained by two suction filtration was combined and dried. 122.9 g of product was obtained, purity: 96%, melting point: 217°C...
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