Ammonia → HCID 57991955, compound

Participants

Reaction Steps

1-(3-Fluoro-4-nitrobenzoyl)thiosemicarbazide (6.6 g, 26 mmol) was dissolved in 30 mL concentrated sulfuric acid and stirred at room temperature for 3 hours. The reaction mixture was poured into a mixture of 40 mL 33% aqueous ammonia and 200 mL ice with stirring. The resulting solution was adjusted to pH 8 with an additional amount of the ammonia solution. An orange solid formed during the process. The product was obtained as a yellow solid after filtering, washing with water, and drying in a vacuum for 24 hours at 50° C. LCMS (API-ES) m/z (%): 241.1 (100%, M++H); 1H NMR (400 MHz, DMSO-d6) δ ppm 7.80 (bs, 3H) 7.93 (d, J=12.32 Hz, 1H) 8.22 (t, J=8.12 Hz, 1H).

Provenance & Evidence