Hydrogen Peroxide → HCID 135899516, compound

Participants

Reaction Conditions

Reaction Steps

H2O2 (70%, 1.2 mL, ca. 24.5 mmol) was added dropwise to a stirred solution of 1-oxide 204 (500 mg, 2.45 mmol) in HOAc (10 mL) and the solution stirred at 50° C. for 24 h. The solution was cooled to 0° C. and the precipitate filtered. The solid was recrystallised from DMF to give 1,4-dioxide 205 (199 mg, 37%) as a red solid: mp>300° C. (235-240° C. dec.); 1H NMR [(CD3)2SO] δ 8.06 (t, J=1.6 Hz, 1H, H-9), 7.86 (br s, 2H, NH2), 7.23 (s, 1H, H-5), 4.77 (t, J=8.3 Hz, 2H, H-8), 3.30-3.60 (m, 2H, H-7); HRMS calcd for C9H8N4O3 (M+) m/z 220.0596, found 220.0601.

Provenance & Evidence