Method for crystallization of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]-ethyl]-1,3-propanediol hydrochloride

摘要

A method for highly efficiently preparing high purity crystals of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chloro-phenyl]-ethyl]-1,3-propanediol hydrochloride. The method involves dissolving 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol in a mixed solvent comprising a solvent in which its hydrochloride is highly soluble and a solvent in which its hydrochloride is less soluble, to prepare a solution of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol; and then adding hydrochloric acid to the resulting solution with stirring, to crystallize the hydrochloride of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chloro-phenyl]ethyl]-1,3-propanediol.

主权项

1. A method for crystallization of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol hydrochloride, comprising:
dissolving 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol in ethanol with heating; then adding ethyl acetate, resulting in a first solution; and adding 1 to 12 mole/L hydrochloric acid to the first solution at a temperature of 50° C. to 90° C. while stirring, resulting a second solution; wherein after crystallization, a system is cooled at a temperature from 0° C. to 30° C. while stirring, resulting crystals are filtered, washed with an additional mixture of ethanol/ethyl acetate and dried under reduced pressure, and the amount of the mixed solvent ranges from 20 to 50 times a mass of said 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol.