Ammonia → HCID 57991878, compound

Participants

Reaction Steps

To a 100 mL round bottom flask was added 1-(phthalazine-5-carbonyl)thiosemicarbazide (0.20 g, 0.81 mmol) and concentrated sulfuric acid (10 mL). The resulting solution was stirred at room temperature for 3 hours. The reaction mixture was poured into a mixture of 10 mL 33% aqueous ammonia and 10 mL ice with stirring. The resulting solution was adjusted to pH 8 with additional ammonia solution. The product was obtained as a yellow solid via filtration and washing with water. The solid was dried in a vacuum oven for 24 hours at 50° C. to provide 5-(phthalazine-5yl)-1,3,4-thiadiazol-2-amine. LCMS (M+H) 230.1 calc. C10H8N5S for 230.0. 1H NMR (400 MHz, CDCl3): δ ppm 8.23 (m, J=8.41 Hz, 1H) 8.46 (d, 1H) 8.53 (d, 1H) 9.63 (d, J=16.24 Hz, 2H). NH2 not detected.

Provenance & Evidence