反应详情

温度

70 °C

Step C (5) [79643-051]: Iodomethane (0.835 mL, 13.4 mmol) was added to a solution of 1-(3-fluoro-4-(5-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (3.21 g, 12.8 mmol) in absolute ethanol (100 mL). The resulting mixture was heated at 70° C. for 3 h. After cooling to rt, the reaction was concentrated in vacuo. The residual volatiles were removed under high vacuum to afford methyl 3-fluoro-4-(5-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydroiodide (4.82 g, 96% yield) as a white solid. LC-MS (M+H)+ 266.0. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.12 (s, 1 H), 7.77 (t, J=8.5 Hz, 1 H), 7.64 (dd, J=11.0, 2.1 Hz, 1 H), 7.37 (dd, J=8.4, 1.4 Hz, 1 H), 2.72 (s, 3 H), 2.36 (s, 3 H).

1. temperatureAfter cooling to rt
2. concentrationthe reaction was concentrated in vacuo
3. customThe residual volatiles were removed under high vacuum