Hydrochloric Acid → HCID 178479162, compound

Participants

Reaction Steps

5-Acetamido-2-amino-4,6-dihydroxypyrimidine (700 g crude) (ex. guanidinium carbonate, diethyl acetamido malonate and ethanol refluxed 48 hours), concentrated hydrochloric acid (2 liters water), (200 ml), were heated to 70° and kept at 70°-75° for 1 hour, then cooled in an ice bath. The product was filtered, washed with HCl (80 ml conc HCl in water 170 ml), then acetone (1 liter), and air dried at 40° to give the title compound (344.5 g). Found: C 24.53, H 4.33, N 28.9 Cl 17.9; C4H6N4O2 ·HCl·H2O requires C 24.4, H 4.6, N 28.5, Cl 18.0%. NMR C13 84.59, 115.24, 157.22 ppm DMSO MS/FAB M+H 143. Vacuum oven drying at 0.5 mm and 85° C. with argon protection gave 320 g (46% yield).

Provenance & Evidence