Sodium Hydroxide → HCID 136065547, compound

Participants

Reaction Conditions

Reaction Steps

N-[1-(3-Amino-2,5-dihydro-5-oxo-1,2,4-triazin-6-yl)ethyl]butyramide (37.0 g) was added to stirred polyphosphoric acid (260 g) at 90° C. over 30 minutes and then the mixture was stirred at 150° C. for 2 h. The mixture was allowed to cool overnight, then warmed to 100° C. and poured into a mixture of ice (370 g) and water (370 g). The solution was adjusted to pH6 by adding 70% sodium hydroxide solution (ca. 230 ml). The precipitated solid was filtered off and was dissolved in 1 N hydrochloric acid (740 ml). The solution was clarrified and adjusted to pH8 by adding 2 N sodium hydroxide solution to give the imidazo[5,1-f]1,2,4-triazin-4(3H)-one as an off-white solid which was filtered off, washed with water, and dried in vacuo at 80° C. Yield=30.2 g; m.p. 266° C.

Provenance & Evidence