A kind of refining process of nalbuphine acid salt
A technology of bukorphine and nalbuphine, which is applied in the field of refining technology of nalbuphine acid salt, can solve the problems of unsatisfactory refining effect, cumbersome method, and small amount of refining, and achieves the reduction of impurity content, simple process, Effect of Yield Improvement
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Embodiment 1
[0031] In reactor, add 55g nalbuphine crude product (6-position hydroxyl β isomer content is 0.25%), then its volume in milliliters is 24 times of the weight in grams of nalbuphine crude product (hereinafter directly The amount of anhydrous methanol represented by W: V) was refluxed at 65° C. to dissolve it, and then 2.7 g of medicinal charcoal was added for decolorization for 15 minutes. Filter, wash the filter cake with anhydrous methanol, combine the washing and filtrate, and concentrate under reduced pressure at 45°C to 3 times the amount of the crude nalbuphine. After natural cooling, put it in a freezer at -5°C for crystallization for more than 8 hours. Filter and dry in vacuum at 45±5°C for 6 hours to obtain 50.0 g of nalbuphine.
[0032] Add 1.25L of purified water to the reaction kettle, add 50.0g of nalbuphine under stirring, heat to 65°C, add dropwise 6M hydrochloric acid to adjust the pH to 3-4, cool down to 45°C after the solid is completely dissolved, add 2.5g of...
Embodiment 2
[0034] Add 60.0g nalbuphine crude product (6-hydroxyl β-isomer content is 0.36%) in the reaction kettle, then use 15 times (W:V) amount of anhydrous methanol, after refluxing at 70°C to dissolve it, add 3g of medicinal charcoal for 15 minutes to decolorize. Filter, wash the filter cake with anhydrous methanol, combine the washing and filtrate, concentrate under reduced pressure at 40±5°C to 2 times (W:V) of the crude nalbuphine, after natural cooling, put it in a freezer at -10°C for crystallization More than 8 hours. Filter and dry in vacuum at 45±5°C for 6 hours to obtain 53.3 g of nalbuphine.
[0035]Add 1.33L of purified water to the reaction kettle, add 53.3g of nalbuphine under stirring, heat to 70°C, add dropwise 6M hydrochloric acid to adjust the pH to 3-4, cool down to 45°C after the solid is completely dissolved, add 2.0g of medicinal charcoal , heat preservation and decolorization for 15 minutes. Filter while hot, and wash the filter cake with purified water. Th...
Embodiment 3
[0037] Add 70.0g (6-hydroxyl β-isomer content is 0.32%) crude product of nalbuphine to the reaction kettle, then use 24 times (W:V) amount of anhydrous methanol, after refluxing at 65°C to dissolve it, add 3.5 g of medicinal charcoal decolorized for 18 minutes. Filter, wash the filter cake with anhydrous methanol, combine the washing and filtrate, concentrate under reduced pressure at 45°C to 3 times the amount of the crude nalbuphine, after natural cooling, stand at -15°C for crystallization for more than 8 hours. Filter, wash the filter cake with anhydrous methanol, suction filter, and vacuum-dry at 45° C. for 6 hours to obtain 63.5 g of nalbuphine.
[0038] Add 1.58L of purified water to the reaction kettle, add 63.5g of nalbuphine under stirring, heat to 65°C, add dropwise 6M hydrobromic acid to adjust the pH to 3-4, cool down to 45°C after the solid is completely dissolved, add 3.2g of drug Using charcoal, keep warm for 18 minutes to decolorize. Filter while hot, and wa...
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