反应详情

温度

190 °C

Add 3-bromo-2-chloro-pyridine (10.08 g, 52.4 mmol) to piperazine (45 g) and piperazine dihydrochloride (83.4 g). Heat the mixture to 190° C. with stirring for one hr. Allow the mixture to cool to about 80° C. then pour the material into water and extract 5 times with DCM. Dry the solution (sodium sulfate), filter and concentrate. Purify using silica gel chromatography, eluting with 15:85 methanol (with 2 M ammonia): DCM to give 1-(3-bromo-pyridin-2-yl)-piperazine as a white solid (8.98 g, 71%).

1. temperatureAllow the mixture to cool to about 80° C.
2. extractionextract 5 times with DCM
3. dry with materialDry the solution (sodium sulfate)
4. filtrationfilter
5. concentrationconcentrate
6. customPurify
7. washeluting with 15:85 methanol (with 2 M ammonia)