反应详情

温度

70 °C

Step U (1): Allyl bromide (0.308 mL, 3.55 mmol) was added to a solution of 1-(2-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (1.0 g, 3.55 mmol, from Preparation B, Step B(4)) in absolute ethanol (25 mL). The resulting mixture was heated at 70° C. for 2 h. After cooling to rt, the reaction was concentrated in vacuo. The residual volatiles were removed under high vacuum to afford allyl 2-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydrobromide (1.45 g, 3.60 mmol, 101% yield) as an off-white solid. LC-MS (M+H)+ 322.0.

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