反应详情

温度

60 °C

To a mixture of 1-(5-amino-3-trifluoromethyl-pyridin-2-yl)-ethanone (408 mg, 2.0 mmol) in 75% sulfuric-acid (6 mL) at 0° C. add sodium nitrite (152 mg, 2.2 mmol) in water (1 mL). Stir the mixture for 30 minutes and add CuBr (343 mg, 2.4 mmol) and 48% HBr (2 mL). Heat the mixture at 60° C. for 30 minutes, cool to 0° C. and basify by dropwise addition of 10M sodium hydroxide. Extract the mixture with ethyl acetate (3×20 mL) and wash the combined organics with brine (50 mL). The organic extract is dried over MgSO4 and the solvent removed under reduced pressure to yield the title compound.

1. temperaturecool to 0° C.
2. extractionExtract the mixture with ethyl acetate (3×20 mL)
3. washwash the combined organics with brine (50 mL)
4. extractionThe organic extract
5. dry with materialis dried over MgSO4
6. customthe solvent removed under reduced pressure