反应详情

N-(3-Cyano-6-fluoro-5-hydroxy-2-methyl[1,1′-biphenyl]-4-yl)-3-hydroxy-2,2-dimethylpropanamide (I-98) (184 mg, 0.54 mmol) was dissolved in toluene (3.7 ml), pyridinium p-toluenesulfonate (34 mg, 0.13 mmol) was added, followed by stirring under heat for 15 hours. After cooling to room temperature, this was diluted with ethyl acetate, washed with aqueous sodium hydrogencarbonate solution 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 recrystallized and purified with diisopropyl ether/ethyl acetate to obtain the entitled compound (118.6 mg, 68%) as a white solid.

1. temperatureunder heat for 15 hours
2. washwashed with aqueous sodium hydrogencarbonate solution and saturated brine
3. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
4. customthe solvent was evaporated away under reduced pressure
5. customThe resulting residue was recrystallized
6. custompurified with diisopropyl ether/ethyl acetate