反应详情

温度

170 °C

To a round bottom flask was added 2,6-dichloropyridin-3-amine (21.4 g, 131 mmol), potassium ethoxy(thioxo)methanethiolate (42.1 g, 262 mmol), and anhydrous NMP (300 mL). The reaction mixture was then heated to 170° C. while stirring in a hot oil bath with a water cooled reflux condenser attached under an atmosphere of nitrogen for 3.5 hours. The crude reaction mixture was then allowed to cool to room temperature, and acidified to pH 5 with glacial acetic acid, which led to a precipitate which was collected by filtration. This precipitate was then suspended in ethyl acetate and washed with water, then brine, dried over sodium sulfate, filtered, and concentrated to give 5-chloro[1,3]thiazolo[5,4-b]pyridine-2-thiol (1-1) as a tan solid. HRMS (M+H)+: observed=202.9502, calculated=202.9499.

1. temperaturecooled
2. temperaturereflux condenser
3. customThe crude reaction mixture
4. temperatureto cool to room temperature
5. filtrationwas collected by filtration
6. washwashed with water
7. dry with materialbrine, dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated