反应详情

Toluene (10 ml), p-toluenesulfonic acid monohydrate (5.3 mg, 28 μmol) were added to N-(5-cyano-2-fluoro-3-hydroxy-6-methylbiphenyl-4-yl)isobutylamide (I-51) (87 mg, 279 μmol), followed by refluxing with a Dean-Stark condenser for 3.5 hours. During the course, p-toluenesulfonic acid monohydrate (5.3 mg, 28 μmol) was added. Alter cooled, ethyl acetate (50 ml) was added to the reaction liquid, the organic layer was successively washed with saturated sodium bicarbonate water (30 ml), saturated brine (30 ml×2), then dried over anhydrous magnesium sulfate, concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain the entitled compound (82 mg, quant.) as a colorless solid.

1. temperatureby refluxing with a Dean-Stark condenser for 3.5 hours
2. temperatureAlter cooled
3. washthe organic layer was successively washed with saturated sodium bicarbonate water (30 ml), saturated brine (30 ml×2)
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)
7. customto obtain the entitled compound (82 mg, quant.) as a colorless solid