Crystallization of (20R,22R)-2-methylene-19-nor-22-methyl-1α,25-dihydroxyvitamin D3 and related precursors
US9212137B2 · kind B2 · utility
1Cited by
4References
33Claims
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Key dates
| Filing date | Mar 14, 2013 |
| Grant date | Dec 15, 2015 |
| Priority date | — |
| Expiry date | Mar 14, 2033 |
Classification
- Technology area (CPC C)Chemistry; Metallurgy
- CPC primaryC07C2602/24
- WIPO fieldOrganic fine chemistry
- WIPO sectorChemistry
Abstract
Disclosed are methods of purifying the compound (20R,22R)-2-methylene-19-nor-22-methyl-1α,25-dihydroxyvitamin D3 to obtain the compound in crystalline form. The methods typically include the steps of dissolving a product containing the compound in a solvent comprising hexane and 2-propanol, cooling the solvent and dissolved product below ambient temperature for a sufficient amount of time to form a precipitate of crystals, and recovering the crystals. Certain diol precursors formed during the synthesis of the compound and its diasteromers also may be obtained in crystalline form using ethyl acetate as a solvent.
Source: USPTO / EPO open patent data. Objective bibliographic and citation counts.