Cyanogen Bromide → HCID 178458301, compound

Participants

Reaction Conditions

Reaction Steps

A partial solution of 4,5-diamino-2-(2-propoxyphenyl)pyrimidin-6-one sulphate (1.1 g), cyanogen bromide (0.33 g), and sodium acetate trihydrate (0.42 g) in 50% aqueous ethanol (44 ml) was stirred at room temperature for 2 hours then allowed to stand overnight. The stirred mixture was then heated in a water bath (temperature 65° C.) for 3 hours, extra cyanogen bromide (0.05 g) added, and the mixture heated for a further 2 hours. The suspension was subjected to partial evaporation under reduced pressure then ammonium hydroxide was added to pH 5. The crude product was collected by filtration and recrystallised from acetonitrile to give the pure title compound, 0.6 g, m.p. 322-335° C. dec. (after melting about 200° C.). NMR (DMSO-d6; 250 MHz) δ: 0.9 (3H, t) ; 1.6 (2H, m) ; 3.9 (2H, t); 6.8 (2H, s); 6.8 (2H, s); 6.9-7.1 (2H, m); 7.3-7.5 (3H, m).

Provenance & Evidence