2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacalciferol in crystalline form

US6835723B2 · kind B2 · utility

Assignee

• Wisconsin Alumni Research Foundation · US

Inventors

• Hector F. DeLuca · Deerfield, US
• James B. Thoden · Madison, US
• Hazel Holden · Fitchburg, US
• Margaret Clagett-Dame · Deerfield, US
• Sumithra Gowlugari · San Mateo, US
• Pawel Grzywacz · Madison, US

Key dates

• Filing date: Dec 12, 2002
• Grant date: Dec 28, 2004
• Expiry date: Apr 22, 2023

Classification

• Technology area (CPC C): Chemistry; Metallurgy
• CPC primary: C07C401/00
• WIPO field: Organic fine chemistry
• WIPO sector: Chemistry

Abstract

A method of purifying 2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacaciferol to obtain 2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacalciferol in crystalline form. The method includes the steps of boiling a solvent such as acetone under inert atmosphere, dissolving a product containing 2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacalciferol to be purified in the solvent, cooling the solvent and dissolved product below ambient temperature for a sufficient amount of time to form a precipitate of 2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacalciferol crystals, and recovering the 2-methylene-19-nor-20(S)-1&agr;-hydroxy-bis-homo-pregnacalciferol crystals.