The condensation of N-(3-hydroxyphenyl)-N-(4-methylphenyl)amine (I) with 2-(chloromethyl)-4,5-dihydro-1H-imidazole (II) by heating at 150-60 C without solvent or in o-dichlorobenzene gives phentolamine as hydrochloride salt (III), which is treated with ammonia to obtain the free base, and finally salified with methanesulfonic acid in ethanol.