Method for preparing clindamycin phosphate
A technology of clindamycin phosphate and dehydroclindamycin is applied in the field of medicine to achieve the effect of reducing the content of impurities and improving the quality of medicines
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Embodiment 1
[0029] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to 100 ml of water, stir to dissolve, add 2.0 g of catalyst palladium carbon after dissolving, pass in hydrogen and keep the hydrogen pressure at 0.4 Mpa, and continue stirring for 1 h. Filter and wash the carbon with a mixed solution of 5ml of water and 40ml of absolute ethanol, combine the filtrate and the carbon washing solution, and add 60ml of absolute ethanol, rotary evaporate at 60°C until about 40ml of liquid remains, then add 50ml of absolute ethanol to it, Continue rotary evaporation at 60°C until a small amount of crystals precipitate, take it out and stir, add 100ml of absolute ethanol dropwise at the same time, cool down to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.
Embodiment 2
[0031] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to a mixed solution of 100 ml water and 20 ml ethanol, stir and dissolve, add catalyst palladium carbon 0.5 g after dissolving, continue to feed hydrogen slowly, and Stir the reaction for 24 hours, filter and wash the carbon with a mixed solution of 5ml of water and 30ml of absolute ethanol, combine the filtrate and the carbon washing solution, and add 60ml of absolute ethanol, and rotary evaporate at 60°C until about 40ml of liquid remains, and then add no Water and ethanol 60ml, continue to rotary evaporate at 60°C until a small amount of crystals are precipitated, take it out and stir, at the same time add 100ml of absolute ethanol dropwise, cool to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.
Embodiment 3
[0033] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to a mixed solution of 100 ml water and 40 ml methanol, stir and dissolve, add catalyst palladium carbon 1.0 g after dissolving, continuously and slowly feed hydrogen, and Stir the reaction for 3 hours, filter and wash the carbon with a mixed solution of 5ml of water and 30ml of absolute ethanol, combine the filtrate and the carbon washing solution, add 60ml of absolute ethanol, and rotate to evaporate at 60°C until about 40ml of liquid remains, then add no Water and ethanol 60ml, continue to rotary evaporate at 60°C until a small amount of crystals are precipitated, take it out and stir, at the same time add 100ml of absolute ethanol dropwise, cool to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.
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