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 (0.55 g, 1.36 mmol) and MeOH (6 mL) is added methane sulfonic acid (0.088 mL, 1.36 mmol). After one hour the solution is concentrated and the solution is treated with Darco-60® for 1 hour, filtered and concentrated to furnish the title compound (0.68 g, 1.36 mmol, >99%). 1H NMR (CDCl3: CD3OD 95:5) δ 0.85 (t, J=7.4 Hz, 6H), 1.67-1.91 (m, 4H), 1.96 (s, 3H), 1.97 (s, 3H), 2.20 (s, 3H), 2.61 (s, 3H), 2.90 (s, 3H), 3.17-3.29 (m, 1H), 7.33 (s, 1H), 7.64 (d, J=7.4 Hz, 1H), 7.89 (d, J=7.9 Hz, 1H), 8.18 (s, 1H), 8.34 (t, J=7.9 Hz, 1H), 9.95 (bs, 1H). LC/MS (m/z): calcd. for C25H32N4O2S2 (M+H)+: 405.6; found: 405.6.

1. concentrationAfter one hour the solution is concentrated
2. additionthe solution is treated with Darco-60® for 1 hour
3. filtrationfiltered
4. concentrationconcentrated