反应详情

温度

70 °C

5,7-Dichloro[1,2,4]triazolo[1,5-a]pyridin-2-amine (Intermediate 15) (0.5 g, 2.46 mmol), cesium carbonate (1.6 g, 4.93 mmol) and pyrazole (0.5 g, 7.39 mmol) was suspended in DMF (10 mL) and stirred at 70° C. for 2 h after which time LCMS showed desired product formation. The reaction mixture was filtered through celite, which was washed with further DMF and the resultant green/brown solution was concentrated in vacuo to give a brown residue, which was partitioned between 10% IPA/DCM (20 mL) and water (10 mL), the organic layer was separated and the aqueous extracted with further 10% IPA/DCM (2×10 mL). The organic layers were combined and dried (MgSO4), filtered and concentrated in vacuo to give the desired product as a brown solid (0.4 g, 69%). 1H NMR (DMSO) δ 9.16 (d, J=2.6 Hz, 1H), 7.99 (d, J=1.4 Hz, 1H), 7.54 (d, J=2.1 Hz, 1H), 7.36 (d, J=2.1 Hz, 1H), 6.72 (dd, J=2.4, 1.9 Hz, 1H), 6.46 (s, 2H). MS: 235.12 [M+H]+.