反应详情

(4-Amino-5-cyano-2-fluoro-6-methylbiphenyl-3-yl)cyclopentanecarboxylate (I-274) (200 mg, 0.83 mmol) was dissolved in xylene (50 ml), then pyridinium p-toluenesulfonate (50 mg) was added, followed by heating under reflux for 18 hours. After cooling to room temperature, the solvent was evaporated away under reduced pressure. The resulting residue was diluted with ethyl acetate, washed with saturated brine. The obtained organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated away under reduced pressure. The resulting residue was purified by preparative TLC (ethyl acetate:n-hexane=1:2, v/v) to obtain the entitled compound (112 mg, 59%) as a colorless amorphous substance.

1. temperatureby heating
2. temperatureunder reflux for 18 hours
3. customthe solvent was evaporated away under reduced pressure
4. additionThe resulting residue was diluted with ethyl acetate
5. washwashed with saturated brine
6. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
7. customthe solvent was evaporated away under reduced pressure
8. customThe resulting residue was purified by preparative TLC (ethyl acetate