Methanesulfonic Acid → HCID 86641693, compound

Participants

Reaction Steps

N-(4-(2-(1,3-Dimethyl-1H-pyrazol-4-yl)pyridin-4-yloxy)-2,5-difluorophenyl)-N′-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide (0.278 g, 0.533 mmol) was dissolved in THF (5 ml) and warmed until reflux. Methanesulfonic acid (0.035 ml, 0.533 mmol) was added. A precipitate immediately formed. The mixture was sonicated for 10 min and allowed to cool to RT. The precipitate was filtered off and dried overnight in the drying pistol (80° C.) to yield N-(4-(2-(1,3-Dimethyl-1H-pyrazol-4-yl)pyridin-4-yloxy)-2,5-difluorophenyl)-N′-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide mesylate (234 mg, 71.1% yie3ld). 1H NMR (400 MHz, DMSO-d6): δ 11.20 (s, 1H), 9.71 (s, 1H), 8.57 (d, 1H), 8.19-8.14 (m, 1H), 7.90 (s, 1H), 7.66-7.62 (m, 1H), 7.58-7.55 (m, 2H), 7.38 (s, 1H), 7.19-7.14 (m, 2H), 7.05-7.02 (m, 1H), 3.79 (s, 3H), 2.34 (s, 3H), 2.29 (s, 3H), 1.68-1.65 (m, 2H), 1.58-1.56 (m, 2H); MS (ESI) m/z: 522.2 (M+H+).

Provenance & Evidence