The present invention relates to a process for the preparation of freeze-dried 2-[(3-aminopropyl)amino]ethanethiol comprising the following steps:a) the reaction of a solution of amifostine with a strong acid, to obtain a solution of 2-[(3-aminopropyl)amino]ethanethiol, andb) the freeze-drying of the solution of 2-[(3-aminopropyl)amino]ethanethiol.