Sodium Carbonate → HCID 54426403, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of the product from Step c (0.7025 g, 1.41 mmol) in ethanol (12 ml) and 2 M aqueous HCl (25 ml) was stirred at 60° C. for 5.5 h. The mixture was then neutralised by adding dropwise saturated aqueous Na2CO3. The resulting precipitate was collected by filtration, washed with water, then hexane, and dried under vacuum at 60° C. This was purified by recrystallisation (MeOH—CH2Cl2), then flash chromatography (silica gel, 3-5% MeOH/CH2Cl2) to afford 0.2044 g (39%) of the title compound as a white solid: mp 208-220° C.; 1H NMR (360 MHz, d6-DMSO) δ5.66 (2 H, s), 7.48-7.49 (3 H, m), 7.58-7.72 (5 H, m), 7.94 (1 H, br s), 8.40 (1 H, s), 8.47 (2 H, d, J=7.2 Hz), 15.10 (1 H, br s); MS (ES+) m/e 370 [MH]+; Anal. Found C, 65.07; H, 4.05; N, 26.01. C20H15N7O.0.1 H2O requires C, 64.72; H, 4.13; N, 26.41%.

Provenance & Evidence