反应详情

A mixture of (2-bromopyridin-4-yl)methanol [118289-16-0] (370 mg, 2.00 mmol), 1H-pyrazole (204 mg, 3.00 mmol), Cu powder (26 mg, 0.40 mmol) and Cs2CO3 (1.30 g, 4.00 mmol) in acetonitrile (4 mL) was heated under reflux for 16 h. The reaction mixture was cooled to rt and concentrated under reduced pressure. The residue was taken up in ethyl acetate and washed with water and brine, dried over anhydrous sodium sulfate, filtered and the organic layer was evaporated under reduced pressure. The residue was purified by flash-column chromatography over silicagel (eluent: 50% ethyl acetate in hexane) to yield the title compound (260 mg, 74%). [LCMS RtF=0.31 min, [M+H]+=176.1].

1. temperaturewas heated
2. temperatureunder reflux for 16 h
3. concentrationconcentrated under reduced pressure
4. washwashed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. customthe organic layer was evaporated under reduced pressure
8. customThe residue was purified by flash-column chromatography over silicagel (eluent: 50% ethyl acetate in hexane)