反应详情

To a solution of 8-(1-ethyl-propyl)-2,6-dimethyl-3-(3-methyl-5-pyridin-2-yl-thiophen-2-yl)-imidazo[1,2-b]pyridazine (0.15 g, 38 mmol) and MeOH (2 mL) is added AcCl (0.028 mL, 0.39 mmol). After one hour the solution is concentrated and the residue recrystallized from EtOAc/hexane furnish the title compound (0.11 g, 0.26 mmol, 69%). 1H NMR (CDCl3), δ 0.97 (t, J=7.4 Hz, 6H), 1.75-2.03 (m, 4H), 2.17 (s, 3H), 2.66 (s, 3H), 2.77 (s, 3H), 3.86-3.98 (m, 1H), 7.17 (s, 1H), 7.21-7.30 (m, 2H), 7.62 (bs, 1H), 7.67-7.7.82 (m, 2H), 8.60 (d, J=4.8 Hz, 1H). LC/MS (m/z): calcd. for C23H26ClN5S (M+H)+: 428.1; found: 391.2.

1. concentrationAfter one hour the solution is concentrated
2. customthe residue recrystallized from EtOAc/hexane