Patent ID: 7880022
Filing Date: 2011-02-01
Classification: C07D

Abstract:
1. A method for separating and purifying 13-dehydroxybaccatin III and 10-deacetylpaclitaxel simultaneously from a taxane-containing material, the method comprising the steps of: (a) extracting the taxane-containing material with at least one organic solvent selected from the group consisting of low-molecular alcohols of C1 to C4 and halogenated alkanes (C1-C2), and concentrating the solvent including the extracted taxane-containing material; (b) partitioning the concentrated solution obtained from step (a) by adding at least one organic solvent selected from the group consisting of halogenated alkanes (C1-C2), ethers, ethyl acetate and butanol, that is not mixable with water, and liquid/liquid extracting the partitioned solution to separate an organic solvent layer of the at least one organic solvent selected from the group consisting of halogenated alkanes (C1-C2), ethers, ethyl acetate and butanol; (c) concentrating the extracted solution obtained from step (b) under reduced pressure, dissolving the concentrated solution in 0.5%(v/v) to 10%(v/v) methanol/dichloromethane mixture solution, and performing normal phase low-pressure liquid chromatography to obtain paclitaxel, 13-dehydroxybaccatin III and 10-deacetylpaclitaxel active fractions at the same time; and (d) as a step of separating and purifying 13-dehydroxybaccatin III and 10-deacetylpaclitaxel from the 13-dehydroxybaccatin III and 10-deacetylpaclitaxel active fractions obtained from the normal phase low-pressure liquid chromatography in step (c), (d-1) dissolving the 13-dehydroxybaccatin III active fraction obtained from the normal phase low-pressure liquid chromatography in step (c) in at least one organic solvent selected from the group consisting of alcohols of C1 to C4, acetonitrile, and purified water, and performing reverse phase low-pressure liquid chromatography to obtain 13-dehydroxybaccatin III active fraction; and (d-2) dissolving the 10-deacetylpaclitaxel active fraction obtained from the normal phase low-pressure liquid chromatography in step (c) in at least one organic solvent selected from the group consisting of alcohols of C1 to C4, acetonitrile, and purified water, and performing reverse phase low-pressure liquid chromatography to obtain 10-deacetylpaclitaxel active fraction.