反应详情

温度

160 °C

To the 3-bromo-6-chloro-7-methyl-imidazo[1,2-b]pyridazine from Part B was added n-BuNH2 (10 ml). The mixture was heated in a microwave at 160° C. for 60 min (30+30 min.). The mixture was concentrated and the residue was subjected to ISCO (40 g column, hexane 3 min., 0-100% EtOAc in hexane over 25 min. the EtOAc 10 min.) to five the titled compound (348 mg). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 0.97 (t, J=7.39 Hz, 3H) 1.29-1.50 (m, 2H) 1.61-1.71 (m, 2H) 2.14 (s, 3H) 3.44 (q, J=6.62 Hz, 2H) 4.39 (br. s., 1H) 7.34 (s, 1H) 7.37 (s, 1H). LRMS (ESI) m/z 283 and 285 [(M+H)]+, calc'd for C11H15BrN4: 283.17.

1. concentrationThe mixture was concentrated
2. custom40 g column, hexane 3 min., 0-100% EtOAc in hexane
3. customover 25 min.
4. customthe EtOAc 10 min.