公开(公告)号：US06432936B1

公开(公告)日：2002-08-13

申请号：US09233738

申请日：1999-01-20

申请人： Hector F. DeLuca ,  Rafal R. Sicinski ,  Hazel Holden ,  James Brian Thoden

发明人： Hector F. DeLuca ,  Rafal R. Sicinski ,  Hazel Holden ,  James Brian Thoden

IPC分类号： A61K31592

CPC分类号： C07C401/00

摘要： A method of purifying 1&agr;-hydroxyvitamin D2 to obtain 1&agr;-hydroxyvitamin D2 in crystalline form. The method includes the steps of boiling a solvent selected from the group consisting of ethyl formate, ethyl acetate and a 2-propanol-hexane mixture under inert atmosphere, dissolving a product containing 1&agr;-hydroxyvitamin D2 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 1&agr;-hydroxyvitamin D2 crystals, and recovering the 1&agr;-hydroxyvitamin D2 crystals. Optionally, petroleum ether may be added to the solvent after dissolving the product to be purified in the solvent.

摘要翻译： 一种纯化1α-羟基维生素D2以获得结晶形式的1α-羟基维生素D 2的方法。 该方法包括在惰性气氛下沸腾选自甲酸乙酯，乙酸乙酯和2-丙醇 - 己烷混合物的溶剂的步骤，将待纯化的含有1α-羟基维生素D2的产物溶解于其中。 溶剂，将溶剂和溶解的产物在环境温度以下冷却足够的时间以形成1α-羟基维生素D2晶体的沉淀物，并回收1α-羟基维生素D 2晶体。 任选地，在将要纯化的产物溶解在溶剂中之后，可以将石油醚加入到溶剂中。

公开(公告)号：US06462031B2

公开(公告)日：2002-10-08

申请号：US09738483

申请日：2000-12-15

申请人： Hector F. DeLuca ,  Rafal R. Sicinski ,  Hazel Holden ,  James Brian Thoden

发明人： Hector F. DeLuca ,  Rafal R. Sicinski ,  Hazel Holden ,  James Brian Thoden

IPC分类号： A61K31592

CPC分类号： C07C401/00

摘要： A method of purifying 1&agr;-hydroxyvitamin D2 to obtain 1&agr;-hydroxyvitamin D2 in crystalline form. The method includes the steps of boiling a solvent selected from the group consisting of ethyl formate, ethyl acetate and a 2-propanol-hexane mixture under inert atmosphere, dissolving a product containing 1&agr;-hydroxyvitamin D2 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 1&agr;-hydroxyvitamin D2 crystals, and recovering the 1&agr;-hydroxyvitamin D2 crystals. Petroleum ether is also added to the solvent after dissolving the product to be purified in the solvent.

摘要翻译： 一种纯化1α-羟基维生素D2以获得结晶形式的1α-羟基维生素D 2的方法。 该方法包括在惰性气氛下沸腾选自甲酸乙酯，乙酸乙酯和2-丙醇 - 己烷混合物的溶剂的步骤，将待纯化的含有α-羟基维生素D2的产物溶解在溶剂中，冷却溶剂 并将产物低于环境温度溶解足够的时间以形成1α-羟基维生素D2晶体的沉淀物，并回收1α-羟基维生素D 2晶体。 将待纯化的产物溶解在溶剂中之后，也将石油醚加入到溶剂中。