反应详情

温度

70 °C

Step Q (3): Iodomethane (1.43 mL, 22.9 mmol) was added to a solution of 1-(3-fluoro-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (5.48 g, 21.8 mmol) in absolute ethanol (200 mL). The resulting mixture was heated at 70° C. for 3 h. After cooling to rt, the reaction was chilled at −20° C. for 2 h. The precipitate was collected by vacuum filtration. The solid was dried under high vacuum to afford methyl 3-fluoro-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydroiodide (8.40 g, 21.4 mmol, 98% yield) as an off-white solid. LC-MS (M+H)+ 266.1. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.91 (d, J=2.4 Hz, 1 H), 7.91 (t, J=8.5 Hz, 1 H), 7.64 (dd, J=11.7, 2.0 Hz, 1 H), 7.35 (d, J=7.3 Hz, 1 H), 2.70 (s, 3 H), 2.38 (s, 3 H).

1. temperatureAfter cooling to rt
2. temperaturethe reaction was chilled at −20° C. for 2 h
3. filtrationThe precipitate was collected by vacuum filtration
4. customThe solid was dried under high vacuum