Water → HCID 24753685, compound

Participants

Reaction Steps

Oxone (0.12 g, 0.07 mmol) was added in one portion to a stirred solution of 2-isopropyl-4-(5-methyl-1H-pyrazol-3-ylamino)-7-(2-methylsulfanyl-ethylsulfanyl)-2H-phthalazin-1-one (0.013 g, 0.03 mmol) in a 4:1 mixture of dioxane/water (1.2 ml) and the reaction mixture was stirred at RT for 1 hour. The reaction mixture was diluted with water (5 ml) and the solution was extracted with EtOAc (3×75 ml), the organic layers were combined, dried (MgSO4), filtered and concentrated under vacuum to give the title compound (0.008 g, 57% yield) as a white solid. δH (400 MHz, DMSO) 9.69 (1H, br s), 8.75 (1H, d), 8.71 (1H, d), 8.47 (1H, dd), 6.40 (1H, s), 5.31-5.22 (1H, m), 3.95-3.89 (2H, m), 3.48-3.42 (2H, m), 3.06 (3H, s), 2.29 (3H, s), 1.36 (6H, d) Tr=1.61 min, m/z (ES+) (M+H)+ 454.10.

Provenance & Evidence