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US 12,209,107 B2Granted
Process for preparing high puritiy allopregnanolone and intermediates thereof
AssigneeCrystal Pharma, S.A.U.
InventorsIvano Messina, Jesús Miguel Iglesias Retuerto, Ana María Ares Sacristán
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Abstract
The invention relates to an efficient and industrially applicable process for the preparation and purification of allopregnanolone and intermediates thereof without the assistance of column chromatography.
Claims16
A chromatography-free process for preparing allopregnanolone which comprises:
- reacting isoallopregnanolone with a strong carboxylic acid having a pKa≤3 under suitable Mitsunobu conditions, thereby obtaining a 3-carboxylic ester of allopregnanolone;
- precipitating the 3-carboxylic ester of allopregnanolone in a solvent system comprising water and an organic solvent;
- purifying the precipitate of the 3-carboxylic ester of allopregnanolone by recrystallizing in a non-polar solvent;
- and
- subjecting the purified 3-carboxylic ester of allopregnanolone to hydrolysis, thereby obtaining allopregnanolone.
2 more elements
Dependencies are inferred from the claim text.