Hydrochloric Acid → 2-amino-4-oxo-7-(thiophen-3-ylmethyl)-3,5-dihydropyrrolo[3,2-d]pyrimidine-6-diazonium;chloride

Participants

Reaction Conditions

Reaction Steps

Charged 23.4 kg (74.1 mol) of 2,6-diamino-3,5-dihydro-7-(3-thienylmethyl)-4H-pyrrolo[3,2-d]pyrimidin-4-one, hydrochloride, monohydrate (U.S. Pat. No. 4,923,872), 240 L water and 14.9 kg (147.1 mol) 36% hydrochloric acid to a nitrogen-purged 800 L reactor. The resulting slurry is cooled to 0° C. A solution of 7.9 kg (114.5 mol) sodium nitrite in 20 L water is added to the slurry over 40 minutes. The reaction mixture is heated to 20° C. and held at that temperature for 1.3 hours. The product is collected and washed with 90 n water yielding 63.5 kg of the title compound as a water wet cake.

Provenance & Evidence