Ammonia → HCID 5329597, compound

Participants

Reaction Steps

To a strirred suspension of 2,6-diamino-5-nitroso-4-cyclohexylmethoxypyrimidine (0.10 g, 0.4 mmol) in water (5 ml) at 50° C. was added sodium dithionite (0.16 g, 0.92 mmol) in portions over a period of 5 h. The reaction mixture was allowed to cool to room temperature and stirred at ambient temperature overnight. The pH of the solution was adjusted to 7 with aqueous ammonia solution (2 ml), and the resulting fine yellow precipitate was collected by filtration and washed with water. The product was purified by recrystallisation from water (0.06 9, 60%), m.p. 154° C.; (Found: C, 55.50; H, 7.95; N, 29.34% C11H19N5O requires C, 55.69; H, 8.02; N, 29.53%); δH (200 MHz, d6-DMSO) 1.02-1.39 (5H, m, C6H11), 1.71-1.89 (6H, m, C6H11), 3.22 (2H, br s, NH2), 4.03 (2H, d, OCH2, J=6.53 Hz), 5.32 (2H, br s, NH2), 5.71 (2H, br s, NH2); m/z (+EI) 237 (M+, 84%), 155 (MH+-C7H13, 100), 124 (MH+-C7H13O, 15).

Provenance & Evidence