反应详情

温度

150 °C

A solution of Example 113E (0.194 g, 0.488 mmol) and 4-bromo-1H-pyrazole (0.115 g, 0.781 mmol) in 1-methyl-2-pyrrolidinone (0.8 mL) was treated with potassium carbonate (0.169 g, 1.22 mmol), and the reaction was heated at 150° C. for 2.5 hours. The reaction was cooled to ambient temperature, and partitioned between water and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The concentrate was purified by flash chromatography on a silica gel column, eluting with a gradient of 0% to 1% methanol in dichloromethane, to provide the title compound. MS ESI(+) m/z 509.0 [M+H]+.

1. temperatureThe reaction was cooled to ambient temperature
2. custompartitioned between water and ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe concentrate was purified by flash chromatography on a silica gel column
8. washeluting with a gradient of 0% to 1% methanol in dichloromethane