Hydralazine Hydrochloride → 1-Chlorophthalazine

In another major embodiment of this invention, a process of preparing pure hydralazine hydrochloride is disclosed, comprising the steps of: a) reacting phthalazinone with phosphorous oxychloride at a specific temperature to produce 1-chlorophthalazine salt; b) concentrating the reaction mixture by distillation; c) isolating the 1-chlorophthalazine salt concentrated in step (b) by precipitating 1-chlorophthalazine salt through the addition of a mineral add in the presence of a solvent, filtering the resulting solid precipitated 1-chtorophthalazine salt, and drying; d) reacting the isolated and dried 1-chlorophthalazine salt with hydrazine hydrate without any substantial amount of organic solvent present and precipitating the resulting hydralazine base by adding a solvent; e) purifying the hydralazine base in a non-aqueous medium; f) converting the purified hydralazine base to hydralazine hydrochloride in a non-aqueous medium, and isolating the same; and g) purifying the isolated hydralazine hydrochloride by dissolving hydralazine hydrochloride in hot water to make a solution, treating the solution with a color adsorbent and a chelating agent, filtering off the adsorbent and chelating agent, adjusting the pH of the solution using a base or acid, and precipitating hydralazine hydrochloride by adding a water miscible solvent at a lower temperature.

ORD-Eintrag

ord-cde05009d96a42d1a6ba458a5e365b2a

Quelldatensatz

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07807830B2