反应详情

温度

70 °C

Aqueous 20% (w/v) potassium carbonate solution (9.0 ml, 13.0 mmol) was added to a methanol (9 ml) suspension of N-(5-cyano-2-fluoro-3-methoxy-6-methylbiphenyl-4-yl)-2,2,2-trifluoroacetamide (I-37) (400 mg, 1.14 mmol), followed by stirring at 70° C. for 16 hours. The reaction liquid became uniform with temperature elevation. The reaction liquid was cooled to room temperature, methanol was evaporated away under reduced pressure, water was added to the residue, followed by extraction twice with ethyl acetate, the organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate. After nitration and concentration under reduced pressure, the entitled compound (266 mg, 91%) was obtained as a white solid.

1. customThe reaction liquid
2. customThe reaction liquid
3. temperaturewas cooled to room temperature
4. custommethanol was evaporated away under reduced pressure, water
5. additionwas added to the residue
6. extractionfollowed by extraction twice with ethyl acetate
7. washthe organic layer was washed with saturated brine
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationAfter nitration and concentration under reduced pressure