反应详情

温度

70 °C

Step T (4) [80456-011]: Iodomethane (0.281 mL, 4.51 mmol) was added to a solution of 1-(4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-3-fluorophenyl)thiourea (1.14 g, 4.30 mmol) in absolute ethanol (50 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 4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-3-fluorophenylcarbamimidothioate, hydroiodide (1.76 g, 4.32 mmol, 101% yield) as a grey solid. LC-MS (M+H)+ 280.1.

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