反应详情

温度

70 °C

Aqueous potassium carbonate solution (1.25 ml) [potassium carbonate (15 g) was dissolved in water (100 ml)] and methanol (1.25 ml) were added to N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide (I-38) (133 mg, 0.322 mmol), followed by stirring overnight at 70° C. After cooling, methanol was evaporated away under reduced pressure, followed by extraction with ethyl acetate, washing with saturated brine and drying on anhydrous magnesium sulfate, the solvent was concentrated under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1) to obtain the entitled compound (95 mg, 94%) as a colorless solid.

1. temperatureAfter cooling
2. custommethanol was evaporated away under reduced pressure
3. extractionfollowed by extraction with ethyl acetate
4. washwashing with saturated brine
5. dry with materialdrying on anhydrous magnesium sulfate
6. concentrationthe solvent was concentrated under reduced pressure
7. customto obtain a pale brown residue
8. customThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)