反应详情

Potassium thiocyanate (16.0 g, 165 mmol) and 6-chloropyridin-3-amine (2.6 g, 20.2 mmol) were dissolved in acetic acid (52 mL). To this solution was added dropwise a solution of bromine (3.2 mL, 62.5 mmol) in acetic acid (12 mL) under cooling in a water bath, and the mixture was stirred for 2 hr. The mixture was warmed to, stirred for 10 hr, and water (30 mL) was added. This reaction mixture was filtered at 85° C., and the insoluble material was suspended in acetic acid (50 mL) and the suspension was filtered. The obtained filtrate was neutralized with aqueous ammonia solution, and the precipitated solid was collected by filtration and recrystallized from methanol to give the title compound (2.0 g, 54%) as a colorless powder.

1. temperatureunder cooling in a water bath
2. temperatureThe mixture was warmed to,
3. stirringstirred for 10 hr
4. filtrationThis reaction mixture was filtered at 85° C.
5. filtrationthe suspension was filtered
6. filtrationthe precipitated solid was collected by filtration
7. customrecrystallized from methanol