反应详情

温度

70 °C

Step B (5): Iodomethane (0.184 mL, 2.95 mmol) was added to a solution of 1-(2-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (664 mg, 2.36 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 2-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydroiodide (1.05 g, 105% yield) as a white solid. LC-MS (M+H)+ 296.2. 1H NMR (500 MHz, methanol-d4) δ ppm 7.70 (s, 1 H) 6.57 (d, J=10.68 Hz, 1 H) 6.12 (d, J=6.41 Hz, 1 H) 2.74 (s, 3 H) 1.50 (s, 3 H) 1.17 (s, 3 H).

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