Ammonium Hydroxide → HCID 14503124, compound

Participants

Reaction Steps

To an ice-cold 5.25% sodium hypochlorite solution (33.8 mL) was added 7N NH4OH (17.8 mL) and stirred for 10 minutes. A solution of 2-aminopurine-6-thione 1, see A. G. Beaman and R. K. Robins, J. Am. Chem. Soc., 83, 4038, (1961), (1.67 g, 22 mmol) in 2N KOH (11 mL) was added and continued stirring for 25 min at 0.C. The mixture was allowed to stand at 0° C. without stirring for 1.5 h. The precipitate was collected by filtration and washed with small amount of water and EtOH to obtain 1.45 g (36%) of the title compound, mp>250° C.: UV: λmax (pH 1) 325 nm (ε 6,400), 240 nm (sh): λmax (pH 7) 310 nm (ε 5,900), 237 nm (ε 6,800): λmax (pH 11) 312 nm (ε 5,900): 1H NMR (DMSO-d6): δ 5.78 (br s, 2, NH2, exchangeable in D2O), 7.73 (s, 1, C8H): Anal. Calcd for C5H6N6S.1/2 H2O (191.1): C, 31.41: H, 3.27: N, 43.98: S, 16.79. Found: C, 1.89: H, 3.27: N, 43.38: S, 17.19.

Provenance & Evidence