反应详情

温度

100 °C

A heterogeneous mixture of 1-(4-bromopyridin-2-yl)-4-isopropylsemicarbazide (0.315 g, 1.15 mmol) in phosphorous oxychloride (1.06 mL, 11.5 mmol) was heated at 100° C. for 2 h. The homogenous solution was allowed to cool to RT. Toluene (10 mL) was added and removed in vacuo (3×). DCM (20 mL) and saturated sodium bicarbonate (aq.) was added to the solid and stirred. The off-white solid was collected by filtration and washed with DCM to give 7-bromo-N-isopropyl-[1,2,4]triazolo[4,3-a]pyridin-3-amine. MS (ESI, pos. ion) m/z: 255.2 (M+1).

1. temperatureto cool to RT
2. customremoved in vacuo (3×)
3. additionDCM (20 mL) and saturated sodium bicarbonate (aq.) was added to the solid
4. filtrationThe off-white solid was collected by filtration
5. washwashed with DCM