Hydrochloric Acid → HCID 178420058, compound

Participants

Reaction Conditions

Reaction Steps

The product from Example 3 step b) (0.3 g) was suspended in ethanol (10 ml) with 2 N hydrochloric acid (21 ml) and heated at 65° C. for 5.5 h. Saturated sodium carbonate solution was added dropwise until a solid precipitated and this was collected by filtration and washed several times with water in the sinter funnel. The solid was recrystallised from methanol to give the required product (0.115 g, m.p. 255° C.). 1H NMR (360 MHz, DMSO) δ 5.64 (2H, s), 7.50 (3H, m), 7.62 (2H, m), 8.08 (1H, s), 8.16 (1H, s), 8.84 (1H, s), 8.90 (1H, s), 9.85 (1H, s); MS (ES+) m/e 372 [MH+]. Anal. Found C, 58.21; H, 3.53; N, 33.95. C18H13N9O requires C, 58.16; H, 3.26; N, 33.39%.

Provenance & Evidence