The reaction of (2-hydroxyethyl)hydrazine (I) with MsCl in pyridine gives the trimesylated compound (II), which is treated with LiCl in refluxing acetone to yield 1-(2-chloroethyl)-1,2-bis(methanesulfonyl)hydrazine (III) (1). Finally, this compound is condensed with methyl isocyanate (IV) by means of TEA in acetonitrile to afford the target semicarbazide.