反应详情

A mixture of N-(5-cyano-2-fluoro-3,3′-dihydroxy-6-methylbiphenyl-4-yl)isobutylamide (I-56) (60 mg, 0.183 mmol), p-toluenesulfonic acid monohydrate (10.4 mg, 0.0548 mmol) and toluene (5 ml) was heated under reflux for 2.5 hours. After cooling, this was diluted with ethyl acetate, successively washed with 1 N hydrochloric acid and saturated brine, dried on anhydrous magnesium sulfate, the solvent was evaporated away under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain the entitled compound (30.9 mg, 54%) as a pale yellow solid.

1. temperaturewas heated
2. temperatureunder reflux for 2.5 hours
3. temperatureAfter cooling
4. washsuccessively washed with 1 N hydrochloric acid and saturated brine
5. dry with materialdried on anhydrous magnesium sulfate
6. customthe solvent was evaporated away 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=4:1)