High-purified tropisetron hydrochloride compound
A technology of tropisetron hydrochloride and tropisetron, which is applied in the field of medicine, can solve the problems of low purity of finished products and affect the safety of pharmaceutical preparations, and achieve the effects of high yield, low cost and optimized product quality
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Embodiment 1
[0017] The refining of embodiment 1 tropisetron hydrochloride
[0018] (1) 50g tropisetron hydrochloride crude product is dissolved in 500ml water, then slowly add 10% (g / ml) sodium carbonate solution, stir and react until the solution pH is 8, produce tropisetron precipitation, filter, 50 ℃ Drying under reduced pressure gave 41.7 g of tropisetron.
[0019] (2) Dissolve 41.7 g of Tropisetron obtained in the previous step in 300 ml of n-butanol, add 3.5 g of activated carbon, stir at room temperature for 35 minutes, filter for decarburization, and collect the filtrate.
[0020] (3) The filtrate obtained in the previous step is separated and purified by a preparative chromatographic column to obtain creatine sodium phosphate refined product, wherein the mobile phase used in the chromatographic column is dichloromethane and volume accounting for 65% of mobile phase by volume Hydrochloric acid aqueous solution with a pH of 1; the stationary phase filler is silica gel; the flow ra...
Embodiment 2
[0027] The refining of embodiment 2 tropisetron hydrochloride
[0028] (1) 50g tropisetron hydrochloride crude product is dissolved in 500ml water, then slowly add the sodium hydroxide solution of 8% (g / ml), stirring reaction is 9 to solution pH, produces tropisetron precipitation, filters, 40 °C and dried under reduced pressure to obtain 41.3 g of tropisetron.
[0029] (2) Dissolve 41.3 g of Tropisetron obtained in the previous step in 300 ml of n-hexane, add 3.3 g of activated carbon, stir at room temperature for 45 minutes, filter for decarburization, and collect the filtrate.
[0030] (3) The filtrate obtained in the previous step is separated and purified by a preparative chromatographic column to obtain creatine sodium phosphate refined product, wherein the mobile phase used in the chromatographic column is dichloromethane whose volume accounts for 45% of the mobile phase and 55% dichloromethane whose volume accounts for the mobile phase Hydrochloric acid aqueous soluti...
Embodiment 3
[0037] The refining of embodiment 3 tropisetron hydrochloride
[0038] (1) 50g tropisetron hydrochloride crude product is dissolved in 500ml water, then slowly add the sodium bicarbonate solution of 12% (g / ml), stirring reaction is 7 to solution pH, produces tropisetron precipitation, filters, 40 °C and dried under reduced pressure to obtain 42.0 g of tropisetron.
[0039] (2) Dissolve 42.0 g of Tropisetron obtained in the previous step in 300 ml of n-hexane, add 3.2 g of activated carbon, stir at room temperature for 40 minutes, filter for decarburization, and collect the filtrate.
[0040] (3) The filtrate obtained in the previous step is separated and purified by a preparative chromatographic column to obtain creatine sodium phosphate refined product, wherein the mobile phase used in the chromatographic column is dichloromethane and volume accounting for 60% of mobile phase by volume Hydrochloric acid aqueous solution with a pH of 1; the stationary phase filler is silica g...
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