Ammonia → HCID 13359830, compound

Participants

Reaction Steps

With stirring, 1.4 g. of 4-(2-chlorophenyl)-1,6-dihydro-1,3-dimethyl-7-(2-propynylamino)pyrazolo[3,4-e][1,4]-diazepine is dissolved in a solution of 1 mg. of mercuric oxide in 5 ml. of concentrated sulfuric acid at 50° C. The solution is allowed to stand for 16 hours at room temperature (20°-30° C.), then is poured over crushed ice and basified with excess concentrated aqueous ammonia. The mixture is extracted repeatedly with dichloromethane. The extracts are combined, dried and evaporated at reduced pressure to give a residue of 4-(2-chlorophenyl)-1,6-dihydro-1,3,9-trimethylimidazo-[1,2-a]pyrazolo[4,3-f][1,4]diazepine; m.p. 189-190° C. (dec.) after sublimation at 130° C. and 0.1 mm. Hg.

Provenance & Evidence