Methanesulfonic Acid → HCID 86641692, compound

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Reaction Steps

1-(5-Chloro-2-fluoro-4-(2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yloxy)phenyl)-3-(2-(4-fluorophenyl)acetyl)urea (0.146 g, 0.293 mmol) was fully dissolved in a mixture of THF (4 ml), acetonitrile (4 mL), and methanol (0.5 mL). Methanesulfonic acid (19 μl, 0.293 mmol) was added, and after stirring for several minutes a precipitate started to form. The mixture was stirred at RT for 5 hours. 1-(5-Chloro-2-fluoro-4-(2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yloxy)phenyl)-3-(2-(4-fluorophenyl)acetyl)urea mesylate salt was obtained by suction filtration and was washed with acetonitrile (0.148 g, 82% yield). 1H NMR (500 MHz, DMSO-d6): δ 11.33 (s, 1H), 10.97 (s, 1H), 8.59 (m, 2H), 8.46 (d, 1H), 8.26 (s, 1H), 7.74 (d, 1H), 7.65 (s, 1H), 7.36 (m, 2H), 7.17 (m, 3H), 3.92 (s, 3H), 3.77 (s, 2H), 2.33 (s, 3H); MS (ESI) m/z: 498.1 (M+H+).

Provenance & Evidence