反应详情

N-(4-Acetyl-2-cyano-5-fluoro-6-hydroxy-3-methylphenyl)cyclopropanecarboxamide (I-81) (200 mg, 0.72 mmol) was dissolved in toluene (4 ml), pyridinium p-toluenesulfonate (40 mg, 0.14 mmol) was, added, followed by heating under reflux for 21 hours. After cooling to room temperature, this was diluted with ethyl acetate, washed with water and saturated brine. The obtained organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure. The resulting residue was subjected to silica gel column chromatography, eluted with a mixed solvent of n-hexane/ethyl acetate (3:1, v/V) to obtain the entitled compound (133 mg, 71%) as a white solid.

1. additionadded
2. temperatureby heating
3. temperatureunder reflux for 21 hours
4. washwashed with water and saturated brine
5. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
6. customthe solvent was evaporated away under reduced pressure
7. washeluted with a mixed solvent of n-hexane/ethyl acetate (3:1