Buagafuran Active Pharmaceutical Ingredient, Preparation Method and Application Thereof
AssigneeBei Jing Yuan Qi Zhi Yao Technology Co. Ltd
InventorBo SONG
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Abstract
A method suitable for large-scale production of buagafuran active pharmaceutical ingredient. A buagafuran active pharmaceutical ingredient (API) with a high purity prepared by the method includes an active ingredient of buagafuran, an impurity A, and an impurity B. In the buagafuran API, a content of the active ingredient of buagafuran is higher than 97.5%, and a total content of the impurity A and the impurity B is less than 0.04%. The buagafuran API can be applied to new drug development processes such as clinical research, pharmaceutical research and quality control research.
Claims10
A buagafuran active pharmaceutical ingredient (API), comprising:
- an active ingredient of buagafuran, impurity A and an impurity B, respectively having the following structures:
- wherein, in the buagafuran API, a content of the active ingredient of buagafuran is higher than 97.5%, and a total content of the impurity A and the impurity B is less than 0.04%;
- and
- a method of preparing the buagafuran API comprises the following steps:
- step a:
- obtaining a compound 5 from a compound 4;
- and
- step b:
- obtaining buagafuran from the compound 5;
- wherein, structures of the compound 4, the compound 5 and the buagafuran are:
- wherein, the step a comprises adding the compound 4 to a potassium hydroxide aqueous solution, heating and stirring, then cooling after a reaction is completed to obtain a first mixture, and adding a concentrated hydrochloric acid to adjust a pH of the first mixture to near-neutral, and then performing extraction, drying, filtration and filtrate concentration;
- and
- the step b comprises dissolving the compound 5 in tert-butanol to obtain a second mixture, adding the second mixture to a potassium hydroxide aqueous solution, heating and stirring, adding bromobutane to obtain a third mixture, adjusting a pH of the third mixture to near-neutral, filtering the third mixture to obtain a filtrate, concentrating the filtrate to obtain a concentrate, dissolving the concentrate in methanol, adding sodium borohydride, stirring to obtain a fourth mixture, adding n-hexane and water to adjust a pH of the fourth mixture to acidity, separating out a n-hexane layer, and concentrating to obtain a crude buagafuran.
A method of preparing a buagafuran active pharmaceutical ingredient (API), comprising the following steps:
- step a:
- obtaining a compound 5 from a compound 4;
- and
- step b:
- obtaining buagafuran from the compound 5;
- wherein, structures of the compound 4, the compound 5 and the buagafuran are:
- wherein, the step a comprises adding the compound 4 to a potassium hydroxide aqueous solution, heating and stirring, then cooling after a reaction is completed to obtain a first mixture, and adding a concentrated hydrochloric acid to adjust a pH of the first mixture to near-neutral, and then performing extraction, drying, filtration and filtrate concentration;
- and
- the step b comprises dissolving the compound 5 in tert-butanol to obtain a second mixture, adding the second mixture to a potassium hydroxide aqueous solution, heating and stirring, adding bromobutane to obtain a third mixture, adjusting a pH of the third mixture to near-neutral, filtering the third mixture to obtain a filtrate, concentrating the filtrate to obtain a concentrate, dissolving the concentrate in methanol, adding sodium borohydride, stirring to obtain a fourth mixture, adding n-hexane and water to adjust a pH of the fourth mixture to acidity, separating out a n-hexane layer, and concentrating to obtain a crude buagafuran.
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Dependencies are inferred from the claim text.