Reacción #1978145

Ecuación de reacción

6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol

methylamine

HCl

→

6-methylamino-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol

Rendimiento 58.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturait was cooled to room temperature
2. 2
   FiltraciónThe resulting precipitate was filtered
3. 3
   Lavadowashed with water
4. 4
   Otrodried in vacuo

Procedimiento

6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol (330 mg, 1.77 mmol) was treated with a 40% v/v aqueous solution of methylamine. The reaction mixture was stirred at 100° C. for 17 h, then it was cooled to room temperature and acidified to pH 1-2 with 1 N aqueous HCl. The resulting precipitate was filtered, washed with water, and dried in vacuo to give 185 mg of 6-methylamino-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol as a yellow powder (58% yield): 1H NMR (DMSO-d6): δ 2.83 (d, 3H), 6.85 (d, 1H), 7.44 (broad q, 1H), 7.74 (d, 1H), 14.2 (s, 1H); MS (m/z) 182 [M+H+]+.

Fuente