反应详情

温度

70 °C

Step R (4): Iodomethane (0.413 mL, 6.63 mmol) was added to a solution of 1-(3,5-difluoro-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (1.7 g, 6.31 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 3,5-difluoro-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydroiodide (2.4 g, 5.84 mmol, 92% yield) as a grey solid. LC-MS (M+H)+ 284.0. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.86 (s, 1 H), 7.50 (d, J=8.9 Hz, 2 H), 2.71 (s, 3 H), 2.38 (s, 3 H).

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