Title:
（２０Ｒ，２２Ｒ）−２−メチレン−１９−ノル−２２−メチル−１α，２５−ジヒドロキシビタミンＤ３および関連前駆体の結晶化
Document Type and Number:
Japanese Patent JP6313288
Kind Code:
B2
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.
Inventors:
Deluca Hector F.
Gujiwach Powell
Plum Lory.
Flores Agnitzkaei.
Sorden James Bee.
Holden Hazel M.
Gujiwach Powell
Plum Lory.
Flores Agnitzkaei.
Sorden James Bee.
Holden Hazel M.
Application Number:
JP2015515009A
Publication Date:
April 18, 2018
Filing Date:
April 30, 2013
Export Citation:
Assignee:
Wisconsin Alumni Research Foundation
International Classes:
C07C401/00; C07C29/78; C07C35/32
Foreign References:
| US20110237557 | ||||
| WO2000066548A1 |
Other References:
Journal of Medicinal Chemistry,2012,55,p.4352-4366
Bioorganic & Medicinal Chemistry,2001,9,p.525-535
Bioorganic & Medicinal Chemistry,2001,9,p.525-535
Attorney, Agent or Firm:
Hatsushi Shimizu
Masao Haruna
Hirotaka Yamaguchi
Toshi Gobe
Ryuichi Inoue
Toshimitsu Sato
Koichi Niimi
Tomohiko Kobayashi
Masato Ozeki
Yoshihiro Igarashi
Kazuya Kawamoto
Masao Haruna
Hirotaka Yamaguchi
Toshi Gobe
Ryuichi Inoue
Toshimitsu Sato
Koichi Niimi
Tomohiko Kobayashi
Masato Ozeki
Yoshihiro Igarashi
Kazuya Kawamoto